Agilent Food Testing: Solutions

Application Notebook
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AGILENT FOOD TESTING SOLUTIONS
TABLE OF CONTENTS
Gas Chromatography with Capillary Flow Technology . . . . . . . . . . . . . . . . . . 4
Cost-effective Analysis of Major, Minor and Trace Elements

in Foodstuffs Using the 4100 MP-AES . . . . . . . . . . . . . . . . . . . . . . . . . . 7
Determination of Fatty Acid Methyl Esters (FAMEs) in

Salmon Oil Using Automated Sample Preparation . . . . . . . . . . . . . . . . . . . 11
Method for the Determination of Chemical Contaminants

in Marine Shellfish . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 14
Analysis of Medium Volatility Sulfur Compounds in Coffee

Using Agilent GC/Q-TOF . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 15
Simple, Rapid Analysis of Trace Metals in Foods Using the

Agilent 7700x ICP-MS . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 16
A Reliable and Routine GC/MS/MS Method for the Determination

of Dioxins in Foodstuffs and Animal Feed . . . . . . . . . . . . . . . . . . . . . . . 20
A Prediction Model for Determining Wine Variety using the

Agilent LC/MS Q-TOF and Agilent Mass Profiler Professional . . . . . . . . . . . . . 22
Triple Quadrupole LC/MS Analysis of Aflatoxins in Various Food Samples. . . . . . . 25
Identification and Quantitation of Pesticides in Chamomile and

Ginger Extracts Using an Agilent 6460 Triple Quadrupole LC/MS
system with Triggered MRM . . . . . . . . . . . . . . . . . . . . . . . . . . . . . . 26
Analysis of Plant Stanyl Fatty Acid Esters in Enriched Margarine

Using an Online Coupled Agilent 1220 Infinity LC-7890 GC System. . . . . . . . . . 30
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Published in USA
5991-0348EN
4 Pesticides AGILENT TECHNOLOGIES APPLICATION NOTEBOOK
Gas Chromatography with Capillary Flow Technology

An effective analytical method for detecting pesticide residues in olive oil
DORIS SMITH, KEN LYNAM, Agilent Technologies, Inc., Wilmington, DE, USA
ABSTRACT: The detection of residual organophosphorous (OP) pesticides the MSD:FPD. The CFT device also enabled post-column backflush. Table 1
in processed olive oil is complicated by the chromatographically active lists the chromatographic conditions used for these analyses. Table 2 lists flow
nature of these compounds, which compromises chromatographic resolution. path consumable supplies used in these experiments.
This study demonstrates a quick and effective analytical method for the
Table 1. Chromatographic Conditions
determination of low ppm and trace-level OP pesticide residues in an olive oil
extract. A J&W DB-35ms Ultra Inert (UI) 30 m × 0.25 mm, 0.25 μm column GC/MSD/FPD: Agilent 7890/5975C
resolved the pesticides of interest in less than 16 minutes, yielding excellent Sampler: Agilent 7683B, 5.0 µl syringe
peak shape for even the more problematic OP pesticides. The detection limits CFT device: Purged 2-way splitter
for most of the pesticides were 10–15 ng/mL. A simplified QuEChERS (Quick, Split ratio 1:1 MSD:FPD
Easy, Cheap, Effective, Rugged, and Safe) method provided sufficient sample MSD restrictor: 1.43 m x 0.18 mm id deactivated fused silica tubing
matrix clean-up while preserving low-level analyte detection. A capillary FPD restrictor: 0.53 m x 0.18 mm id deactivated fused silica tubing
flow technology (CFT) device was installed post-column to split the effluent Aux EPC: 3.8 psi constant pressure
between the MSD and FPD and implement an automated backflush to
Column: DB-35ms UI 30 m 0.25 mm 0.25 µm
diminish residual sample carryover and reduce instrument cycle times.
Carrier: Helium, constant pressure 28.85 psi at 95 ºC
INTRODUCTION Inlet: 1 µL, Splitless, 250 ºC
The health benefits of a Mediterranean diet, and of olive oil in particular, Purge flow 60 mL/min at 0.15 min
are widely acknowledged (1, 2). However, as 4 kg of olives are needed to
Gas saver 20 mL/min at 2 min
produce 1 kg of olive oil, residual pesticides can be concentrated in the final
Oven: 95 ºC (0.5 min) to 210 ºC (25 ºC/min),
product and must be monitored to ensure toxic residues do not exceed safe
levels (3). Many common insecticides used in olive tree pest protection belong 10 ºC/min to 250 ºC (0.5 min),
to the organophosphorous (OP) class, and human toxicities for OP pesticides 20 ºC/min to 290 ºC, hold 4.5 min
have shown acute as well as chronic effects from pesticide poisoning (4). OP Postrun backflush: 7.5 min @ 290 ºC
pesticides present a challenge for analysis as they are chromatographically Aux EPC pressure 54 psi during backflush
active compounds that can adsorb onto active sites in the sample flow path, inlet pressure 2 psi during backflush
particularly at trace levels, compromising the analytes’ response. MSD: 300 ºC transfer line, 300 ºC source, 150 ºC quad
Here, we report a sample preparation extraction to detect 16 different FPD: 230 ºC Hydrogen 75 mL/min, Air 100 mL/min
pesticides in olive oil samples, using a procedure based on the evaluation of Carrier + makeup (N2) 60 mL/min
the QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) approach
for the analysis of pesticide residues in the high-lipid olive oil matrix (5). This Table 2. Flow Path Supplies
approach simplifies the traditional, labor-intensive extraction and clean-up Vials: Amber crimp top glass vials (p/n 5183-4496)
procedure, while providing just enough sample matrix clean-up for pesticide Vial Caps: Crimp caps (p/n 5181-1210)
residues analysis. A gas chromatographic system capable of multisignal Vial inserts: 250 μL glass/polymer feet (p/n 5181-8872)
detection can provide complementary data for identification, confirmation, Syringe: 5 μL (p/n 5181-1273)
and quantitation of target analytes from a single injection. This method
Septum: Advanced Green (p/n 5183-4759)
enables simultaneous detection of OP pesticides by gas chromatography with
Inlet liner: Ultra Inert single taper splitless liner with wool
electron ionization mass spectrometry in selective ion monitoring mode (GC/
MS-SIM) and flame photometric detection (FPD) in phosphorus mode by (p/n 5190-2293)
splitting the column effluent 1:1 between the mass selective detector (MSD) Ferrules: 0.4 mm id short; 85/15 vespel/graphite
and FPD. The approach chosen here uses a GC/MSD/FPD system to identify (p/n 5181-3323)
and confirm the order of elution for peaks of interest. The GC/MS system PCT fittings: Internal nut (p/n G2855-20530)
was also equipped with backflush capability. This capability enables faster PCT ferrules: SilTite ferrules, 0.25 mm id (p/n 5188-5361)
instrument cycle time by backflushing late-eluting matrix components back 20x magnifier: 20x Magnifier loop (p/n 430-1020)
through the inlet purge valve.
An analyte protectant (AP) was included in the study methodology to REAGENTS AND CHEMICALS
help minimize the errors caused by matrix-induced signal enhancements– All reagents and solvents were HPLC or Ultra Resi grade. Acetonitrile (ACN)
L-glulonic acid γ-lactone (gulonolactone), was chosen based on the results of from Honeywell (Muskegon, MI, USA), toluene from Burdick & Jackson, and
a previous study examining APs (6). acetone from JT Baker were purchased through VWR International (West
EXPERIMENTAL Chester, PA, USA). The neat pesticide standards were purchased from Chem
An Agilent 7890 GC/5975C MSD equipped with an FPD and 7683B Service, Inc. (West Chester, PA, USA), gulonolactone from Aldrich (St. Louis,
autosampler was used for this series of experiments. A purged two-way MO), and triphenyl phosphate from Alfa Aesar (Ward Hill, MA).
capillary flow technology (CFT) device was used to split the effluent 1:1 to
AGILENT TECHNOLOGIES APPLICATION NOTEBOOK Pesticides 5
SOLUTIONS AND STANDARDS SAMPLE PREPARATION

The 16 target OP pesticides tested for detection were: A sample of extra virgin olive oil was purchased from a local grocery store.
The sample extraction method used a modified QuEChERS approach, as
• Acephate • Dimethoate • Omethoate illustrated in Figure 1. Once the samples were prepared in this way, the
• Azinphos-ethyl • Fenitrothion extract was analyzed by GC/MS/FPD using the chromatographic conditions
• Parathion
in Table 1. Extractions of water and acetonitrile aliquots were prepared in the
• Azinphos-methyl • Fenthion • Parathion-methyl same manner as the samples and served as reagent blanks.
• Carbophenthion • Malathion • Pirimiphos-methyl RESULTS AND DISCUSION
• Chlorpyrifos The 16 targeted OP pesticides were resolved on the Agilent J&W DB-35ms
• Methamidophos
UI 30 m × 0.25 mm, 0.25 μm analysis column in less than 16 minutes.
• Diazinon • Methidathion
The pesticide matrix-matched standard in the Figure 2 chromatogram exhibits
Triphenyl-phosphate (TPP) was used as a surrogate standard.
good separation and peak shape for all of the pesticides.
1 μg/mL and 5 μg/mL spiking solutions were prepared of each of the test
pesticides. TPP was prepared at concentrations of 1, 15, and 100 μg/mL Resolution of 16 Organophosphorus Pesticides
with an Agilent J&W DB-35ms UI Column
in toluene. An analyte protectant solution was prepared by dissolving the
neat gulonolactone in a minimum amount of water and appropriate amount Response
1. Methamidophos 10. Fenitrothion
of ACN to yield a 50 mg/mL concentration. The appropriate amount of

3400000 2. Acephate 11. Parathion
1 3. Omethoate 12. Fenthion
gulonolactone solution was added to the calibration standards to yield a 0.5

3000000 4. Diazinon 13. Methidathion
5. Dimethoate 14. Carbophenthion
2 7 6. Pirimiphos-methyl 15. Triphenyl-phosphate *
mg/mL concentration in each standard.
2600000 5 8-12 7. Parathion-methyl 16. Azinphos-methyl
8. Malathion 17. Azinphos-ethyl
2200000 6 9. Chlorpyrifos *surrogate standard
1800000 13
14
QuEChERS Sample Preparation Workflow 1400000

15
Weigh 3 g sample (± 0.05 g) 50 mL centrifuge tube 1000000

3
4 16
17
600000
Add surrogate standard and QC spike solution if necessary, vortex 1 min 200000
4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00 16.00 17.00
Time
Add 7 mL of of cold DI water and 2 ceramic bars (p/n 5982-9313), Figure 2. GC/FPD chromatogram of a 100 ng/mL matrix-matched OP pesticide
vortex 1 min standard with analyte protectant analyzed on an J&W DB-35ms UI 30 m
× 0.25 mm, 0.25 μm capillary GC column. Chromatographic conditions are
Add 10 mL of ACN, vortex 1 min listed in Table 1.
Add Agilent original QuEChERS extraction salt packet for 10 g samples Chromatography of OP pesticides can be problematic, especially for polar
(p/n 5982-5550) pesticides, often yielding broad peak shapes or excessive tailing, making
reliable quantitation at low levels difficult. The high level of inertness of the
Shake vigorously for 1 min on a mechanical shaker at 1500 rpm DB-35ms UI results in better peak shape and decreased sample adsorption
on active sites within the column, enabling lower detection limits. Figure 3
Centrifuge at 4000 rpm for 5 min depicts the excellent peak shape at 15 ppb for the four polar OP pesticides
with the DB-35ms UI column.
Transfer 8 mL of upper ACN layer to Agilent AOAC dispersive SPE 15 mL tube The analyte protectant used in this analysis, gulonolactone, effectively reduced
for fatty samples (p/n 5982-5158) matrix-related effects and improved the analyte response. Since FPD in
phosphorus mode is selective only to analytes containing phosphorus, it is able
Vortex 1 min, centrifuge at 4000 rpm for 5 min to detect low levels of OP pesticides in complex matrices such as olive oil with
minimal matrix interferences. Excellent signal-to-noise ratios were seen at trace
Transfer upper ACN layer to Agilent AOAC dispersive SPE 15 mL tube levels, indicating a high level of sensitivity.
for fatty samples (Agilent p/n 5982-5158)
The FPD was able to detect OP pesticides down to 10 ng/mL with the
Vortex 1 min, centrifuge at 4000 rpm for 5 min exception of omethoate, diazinon, azinphos-methyl, and azinphos-ethyl,
which were detected at a slightly higher limit of detection of 15 ng/mL. The
Transfer extract to vial and add 0.5 mg/mL analyte protectant detection levels for the targeted OP pesticides were within the maximum
residue levels (MRLs) range of 0.01–2 mg/kg established by the US, EU, and
Analyze extract by GC/MS/FPD Codex Alimentarius for pesticide residues in olives (7-9).
Sample preparation using the QuEChERS approach was effective in retaining
the OP pesticides in the spiked oil sample and providing sufficient clean-up of
Figure 1. Flow chart for the QuEChERS sample preparation procedure for pesticides in the sample matrix for GC analysis. Figure 4 shows an olive oil sample which
olive oil. was fortified with the OP pesticide mix and prepared using QuEChERS. A
blank matrix trace is shown below the analyte trace to indicate the level
of potential matrix interference with the analytes of interest. Peak shapes
for the organophosphorus pesticides are still quite sharp and well-resolved,
indicating excellent performance on the DB-35ms UI column in an olive oil
matrix. The performance of the DB-35ms UI column yielded excellent linearity CONCLUSIONS
over the calibration range of this study. The linearity of the column as defined The Agilent J&W DB-35ms UI capillary column resolved the targeted OP
by the R2 values of the calibration standard curve was ≥ 0.999 for all the pesticides and provided excellent peak shapes for the polar pesticides,
pesticides studied. allowing for more reliable quantitation at low levels. Detection levels for the
OP pesticides in olive oil were at or below the EU, Codex, and US maximum
Recoveries were determined by GC/FPD at the 20, 100, and 500 ng/mL
residue levels for olives. Matrix-matched calibration standards yielded
levels. The recoveries of the pesticides were greater than 70 percent with
regression coefficients R2 ≥ 0.999 and recoveries of fortification studies
RSDs below 10 percent except in the case of acephate, which was slightly
were 63 percent to 107 percent with an average RSD < 9 percent, further
lower with an average recovery of 66 percent.
demonstrating the effectiveness of using the J&W DB-35ms UI columns for
residual pesticide determination.
Excellent Peak Shape for Polar OP Pesticides By splitting the column effluent between the MSD and FPD, selectivity,
on Agilent J&W DB-35ms UI Column
Response identification, and confirmation of OP pesticides from a single injection are
700000 achieved, thereby increasing laboratory productivity. GC/MS-SIM provides
650000
selectivity and confirmation, while further specificity and quantitation is
600000
Methamidophos
achieved by FPD in phosphorus mode. The QuEChERS approach was
550000
Acephate successful at providing just enough sample clean-up to minimize matrix
500000 Dimethoate interferences while still maintaining low-level analyte detection. The simple
450000
QuEChERS extraction method allows for faster sample prep facilitating higher
400000
sample throughput. Residual sample matrix carryover is removed through
350000 Omethoate use of backflush, which eliminates the need for a bakeout cycle, significantly
300000
reducing analytical run times.
250000
200000 This trial successfully demonstrates a quick and efficient analytical method to
150000 monitor low- and trace-level OP pesticide residues in olive oil samples.
100000
3.00 3.50 4.00 4.50 5.00 5.50 6.00 6.50 7.00 7.50 8.00 REFERENCES
Time
Figure 3. Enlarged section of the GC/FPD chromatogram of a 15 ng/mL matrix- (1) J. Brill Bond, Am J Lifestyle Med., 3, p. 44 (2009).
matched pesticide standard with analyte protectant analyzed on an (2) T. Psaltopoulou, A. Naska et al., Am J Clin Nutr., 80, pp. 1012-1018 (2004).
J&W DB-35ms UI capillary column. Chromatographic conditions are
(3) E.G. Amvrazi, T.A. Albanis, J Agric Food Chem., 54, pp. 9642-9651 (2006).
listed in Table 1.
(4) L.G. Sultatos, 43, pp. 271-289 (1994).
GC/FPD Chromatogram of Olive Oil Extract Blank Relative to Spiked sample (5) S.C. Cunha, S.J. Lehotay et al., J Sep Sci., 30, pp. 620-632 (2007).
after Agilent’s QuEChERS extraction and dispersive SPE (6) M. Anastassiades, K. Mastovska et al. J Chromatogr A ., 1015, pp. 163-184
1.
2.
Methamidophos
Acephate
10.
11.
Fenitrothion
Parathion (2003).
3. Omethoate 12. Fenthion
Response
5
4.
5.
Diazinon
Dimethoate
13.
14.
Methidathion
Carbophenthion
(7) The Maximum Residue Limit Database. Available at: http://www.mrldatabase.
7
com. Accessed August 2011.
2600000 6. Pirimiphos-methyl 15. Triphenyl-phosphate *
8-12 7. Parathion-methyl 16. Azinphos-methyl
2400000 8. Malathion 17. Azinphos-ethyl
2200000 1 9. Chlorpyrifos *surrogate standard (8) EU Pesticides Database. Available at: http://ec.europa.eu/sanco_pesticides/
6
public/index.cfm. Accessed August 2011.
2000000 2 13
1800000
15
1600000
14 (9) Codex Maximum Residue Limits. Codex Alimentarius Commission. Available
1400000
1200000
3 4
at: http://www.codexalimentarius.net/pestres/data. Accessed August 2011.
1000000 16
17
800000
100 ng/mL
600000 fortified QC sample
400000
Matrix Blank
200000
3.00 4.00 5.00 6.00 7.00 8.00 9.00 10.00 11.00 12.00 13.00 14.00 15.00
Time
Figure 4. GC/FPD chromatogram of the olive oil extract blank and a 100 ng/mL
fortified olive oil extract both with analyte protectant analyzed on an
J&W DB-35ms UI capillary column. Chromatographic conditions are
listed in Table 1.

Published in USA
AGILENT TECHNOLOGIES APPLICATION NOTEBOOK Metals 7
Cost-Effective Analysis of Major, Minor, and Trace Elements

in Foodstuffs Using the 4100 MP-AES
Tran Nham and Craig Taylor* Agilent Technologies, Melbourne, Australia
* Corresponding author
INTRODUCTION INSTRUMENTATION
Whether the goal is food safety, ensuring quality or establishing provenance, The innovative 4100 MP-AES with its proprietary Microwave Excitation
measuring the trace element content of foods and beverages that we all Assembly is a sequential atomic emission spectroscopic technique capable of
consume is of paramount importance. While some elements are essential for fast, unattended multi-element analysis at varying concentration levels using
our well-being at low concentrations, others like lead and chromium are highly a nitrogen plasma. The unique Microwave Excitation Assembly focuses and
toxic and more still are being linked to viral, neurological and other diseases. contains the microwave energy that is created via a concentrated axial magnetic
Food scares related to contamination or poor quality not only constitute a health field around the torch. This creates a robust toroidal plasma that allows the stable
risk, they also undermine consumer confidence. This can lead to lost earnings introduction of liquid samples. With a central channel temperature of ~5,000
through reduced sales and loss of credibility through adverse publicity. K, MP-AES is highly suited to spectroscopic analysis, as it creates high intensity
atomization emission lines. In addition to simplified spectra, nitrogen-MP-AES
Atomic spectroscopy is well-established for the analysis of metals in foods. The
offers reduced operating costs and increased lab safety compared to flame AA,
technique employed often depends on the requirements of the application in
through the avoidance of costly and highly flammable gases such as acetylene.
terms of elements of interest, expected concentrations, and number and type
of samples. Other important procurement factors that influence instrument The analysis was carried out using an Agilent 4100 MP-AES equipped with a
selection include purchase and operational budget for consumables, gases, standard MP-AES torch, concentric nebulizer, and glass cyclonic spray chamber.
power and labor, as well as service and maintenance costs.
Operating parameters are shown in Table 1.
With lab budgets coming under increasing pressure, Agilent has expanded its
Table 1. Agilent 4100 MP-AES operating parameters
atomic spectroscopy portfolio to include the 4100 Microwave Plasma-Atomic
Emission Spectrometer (MP-AES). MP-AES is a new analytical technique that Instrument parameter Setting
uses a microwave-induced nitrogen plasma to provide elemental analysis, with Nebulizer pressure 160–180 kPa
Read time 3 s (10 s for MDL)
significantly reduced running costs through the use of nitrogen as its plasma gas.
Number of replicates 3 (10 for MDL)
EXPERIMENTAL Stabilization time 15 s
This work describes the analysis of various certified and standard reference Background correction Auto
materials per the sample descriptions below:
METHOD DETECTION LIMITS
• NIES CRM No.7 Tea Leaves: from National Institute of Environmental The Method Detection Limits were determined from the analysis of digested
Studies (NIES), Japan. blank samples. The selected analytical wavelengths and method detection
limits (3σ) are listed in Table 2.
• NIES CRM No.10c Rice Flour: from National Institute of Environmental
Studies (NIES), Japan. Table 2. Agilent 4100 MP-AES element wavelength and method
detection limits (ppb)
• NIST SRM 1577 Bovine Liver: from National Institute of Standards and Element Wavelength (nm) MDL (ppb)
Testing, USA. Al 396.152 0.5
• CRM-Wheat Flour: from High Purity Standards, USA Ba 455.403 0.02
Ca 445.478 14
• CRM-Milk Powder: from High Purity Standards, USA Cd 228.802 1.2
• CRM-Oyster Tissue: from High Purity Standards, USA Co 340.511 4
Cr 425.433 0.5
SAMPLE PREPARATION
Cu 327.396 0.4
A simple acid digestion method was used to prepare three of the samples.
Fe 371.993 3
Initially, 0.25 g of the tea leaves CRM, 0.5 g of bovine liver SRM, and 1 g of
K 769.897 3
rice flour CRM were weighed into separate 250 mL beakers. This was then
K 404.414 280
followed by the addition of 10 mL of HNO3 and each beaker was covered with a
watch glass. The samples were heated on a hot plate until completely dissolved. P 213.618 100
After cooling to room temperature, each digest was transferred to a 100 mL Pb 405.781 5
volumetric flask and made up to the required volume by adding Milli-Q water. Pb 368.343 12
Mg 518.361 4
Pre-prepared sample solutions of CRM-Wheat Flour, CRM-Milk Powder, and CRM- Mn 403.076 0.5
Oyster Tissue in 4% HNO3 were purchased from High Purity Standards, USA. Mo 379.825 1.5
Working standards and a blank were matrix-matched with the samples. Na 589.592 3
Na 568.821 140
Ni 341.476 2
Ni 352.453 2
Sr 407.771 0.01
Zn 213.857 4
8 Metals AGILENT TECHNOLOGIES APPLICATION NOTEBOOK
ANALYSIS OF FOODSTUFFS
Results of the analysis of major, minor and trace extractable elements in six
different foodstuffs are listed in Tables 3 to 8. The measured values (carried
out in triplicate) are in good agreement with the certified values for all CRM
and SRM samples.
Table 3. Results of NIES No.7 Tea Leaves

Element Measured values Certified values
wt% wt%
Ca 0.314 ± 0.013 0.320 ± 0.012
Mg 0.150 ± 0.004 0.153 ± 0.006
K 1.861 ± 0.074 1.86 ± 0.07
mg/kg mg/kg
Ba 5.76 ± 0.57 5.7*
Cd nd 0.03 ± 0.03
Co nd 0.12*
Cr nd 0.15*
Cu 7.13 ± 0.81 7 ± 0.3
Pb nd 0.8 ± 0.03
Ni 6.03 ± 0.63 6.5 ± 0.3
Sr 3.63 ± 0.43 3.7*
Zn 34 ± 3 33 ± 3
* Reference values only
Table 4. Results of NIES No.10c Rice Flour

wt% wt%
Mg 0.127 ± 0.006 0.125 ± 0.008
K 0.279 ± 0.012 0.275 ± 0.010
P 0.300 ± 0.010 0.335 ± 0.008
mg/kg mg/kg
Al 1.49 ± 0.13 1.5*
Ca 95.4 ± 7.0 95 ± 2
Cd 1.83 ± 0.14 1.82 ± 0.06
Co nd 0.007*
Cr nd 0.08*
Cu 4.03 ± 0.32 4.1 ± 0.3
Fe 10..6 ± 0.15 11.4 ± 0.8
Mo nd 1.6 ± 0.1
Ni nd 0.30 ± 0.03
Sr 0.2 0.2*
Zn 21.8 ± 1.0 23.1 ± 0.8
Table 5. Results of NIST 1577 Bovine Liver

wt% wt%
Na 0.247 ± 0.006 0.243 ± 0.013
K 1.00 ± 0.08 0.97 ± 0.06
mg/kg mg/kg
Ca 131 123*
Cd nd 0.27 ± 0.04
Co nd 0.18*
Cu 185 ± 6 193 ± 10
Fe 266 ± 5 270 ± 20
Pb nd 0.34 ± 0.08
Mg 625 ± 45 605*
Mn 10.4 ± 1.41 10.3 ± 1
Mo nd 3.2*
Sr 0.15 ± 0.07 0.14*
Zn 125 ± 4 130 ± 10
Table 6. Results of CRM-Wheat Flour

(mg/kg) (mg/kg)
Al 0.83 ± 0.02 0.85 ± 0.01
Ca 9.64 ± 0.97 9.5 ± 0.1
Cd nd 0.0015*
Co nd 0.001*
Cr 0.013 ± 0.001 0.014*
Cu 0.09 ± 0.008 0.1 ± 0.002
Fe 0.81 ± 0.04 0.90 ± 0.01
K 62.5 ± 0.5 65 ± 0.7
P 61.1 ± 1.7 65 ± 0.7
Pb 0.05 ± 0.001 0.050 ± 0.003
Mg 20.8 ± 0.1 20.0 ± 0.2
Mn 0.36 ± 0.02 0.4 ± 0.008
Ni nd 0.009 ± 0.001
Zn 0.47 ± 0.05 0.50 ± 0.01
Table 7. Results of CRM-Milk Powder Table 8. Results of CRM-Oyster Tissue

Element Measured values Certified values Element Measured values Certified values
(mg/kg) (mg/kg) (mg/kg) (mg/kg)
Al nd 0.020 ± 0.002 Al 2.92 ± 0.07 3*
Ca 131 ± 9 130 ± 1 Ca 15.0 ± 0.49 15*
Co nd 0.0004* Cd nd 0.03*
Cr nd 0.0003* Co nd 0.004*
Cu 0.006 ± 0.001 0.007 ± 0.001 Cr nd 0.007*
Fe 0.018 ± 0.002 0.020 ± 0.001 Cu 0.56 ± 0.05 0.6*
K 178 ± 6 170 ± 2 K 100 ± 0.96 100*
P 98.7 ± 1.3 100 ± 1 P 79.1 ± 0.9 80*
Pb nd 0.002* Pb nd 0.005*
Mg 11.9 ± 0.2 12 ± 0.1 Mg 12.1 ± 0.2 12*
Mn 0.003 ± 0.002 0.003* Mn 0.18 ± 0.01 0.2*
Na 48.7 ± 2.6 50 ± 1 Na 48.9 ± 0.8 50*
Zn 0.48 ± 0.05 0.50 ± 0.01 Ni nd 0.01*
* Reference values only Zn 8.3 ± 0.4 9*
CONCLUSIONS
MP-AES offers any food testing facilities dependent on acetylene-based
instrumentation a real alternative in terms of sensitivity, multi-element
capability, and speed of analysis, while cutting operating costs and improving
the safety of the lab environment through the use of non-flammable nitrogen.
This study shows that following a quick and simple acid digestion sample
preparation procedure (required for three of the six diverse food samples), all
six certified and standard reference materials can be analyzed for trace and
major element concentrations with good accuracy by MP-AES. The addition
of the Agilent 4107 Nitrogen Generator is also possible in order to perform
this analysis with significantly lower gas costs or for analysis in remote
locations where sourcing of gases is costly or difficult.

Published in USA
AGILENT TECHNOLOGIES APPLICATION NOTEBOOK FAMEs 11
Determination of Fatty Acid Methyl Esters (FAMEs) in Salmon Oil

Using Automated Sample Preparation
Norbert Helle and Monika Bzduch, TeLA GmbH Bremerhaven, Rebecca Veeneman, Agilent Technologies, Inc.
INTRODUCTION GC conditions
The automated derivatization of fatty acids (FAs) was performed with the Instrument Agilent 6890 Series GC
Agilent 7696A Sample Prep WorkBench. Since free fatty acids show tailing Column HP 88, 100 m × 250 μm, 0.20 μm
in gas chromatography, transformation of fatty acids into fatty acid methyl Injection volume 2 μL
esters (FAMEs) is widely used. Manual sample derivatization is time-
Injector Split/Splitless, Split 50:1
consuming and may lead to poor repeatibility. Automated derivatization
Carrier gas H2
shows significant enhancement of reproducibility and saves time. Especially
for highly unsaturated fatty acids, slight variations in reaction temperature Temperature-program 70 °C–260 °C
and time can negatively affect repeatability when using manual procedures. Flow 1.4 mL/min
Detector 250 °C, FID
Salmon oil is an excellent source of polyunsaturated omega-3 fatty acids. The
H2 flow: 40 mL/min
two main fatty acids—eicosapentaenoic acid (EPA) and docosahexaenoic
acid (DHA)—have been identified as important health factors and are Air flow: 450 mL/min
correlated with a normal function of the heart. The concentration of EPA Makeup flow, N2: 45 mL/min
and DHA is the crucial quality factor for salmon oil capsules. This application
note demonstrates the use of the Agilent 7696A Sample Prep WorkBench AGILENT WORKBENCH PROGRAM
for derivatization and subsequent determination of both EPA and DHA from
salmon oil capsules. Add 500 μL of TBME to sample
MATERIALS AND METHODS

Mix sample: 3,000 rpm, 3 cycles, bidirectional,
For sample preparation, 10 mg of salmon oil was weighed into a 2-mL
25 seconds
autosampler vial. The sample was diluted in 500 μL of tert-butyl methyl ether
(TBME), using the liquid-dispensing module of the Agilent 7696A Sample Wait for 15 seconds
Prep WorkBench and mixed for 90 seconds with the onboard vortex mixer.
A 250-μL aliquot of the prepared sample was transferred to an empty vial Add 250 μL of sample to empty vial
and 125 μL of a Trimethylsulfoniumhydroxide (TMSH) derivatization solution
[MachereyNagel, Düren] was added and the mixture was again mixed using Add 125 μL of TMSH to empty vial
the vortex mixer of the WorkBench. The mixture was heated for 5 minutes at
80 °C in the single vial heater. The flow diagram for the automated procedure Mix empty vial: 3,000 rpm, 3 cycles, bidirectional
on the Agilent 7696A Sample Prep WorkBench is in shown in Figure 1.
The gas chromatographic conditions were chosen as shown in Table 1. Heat empty vial at 80 °C for 5 minutes
Table 1. GC/FID Conditions Flag empty vial as Result

Peak identification Figure 1. Flow diagram of FAME sample preparation with the Agilent 7696A
C14:0 Myristic acid Sample Prep WorkBench
C16:0 Palmitic acid
C16:1 Palmitoleic acid
C18:0 Stearic acid
C18:1 Oleic acid
C18:2 Linoleic acid
C20:0 Arachidic acid
C18:3 g-Linolenic acid
C20:1 Gadoleic acid
C18:3 Linolenic acid
C22:1 Erucic acid
C20:4 Arachidonic acid
C20:5 Eicosapentaenoic acid
C24:1 Nervonic acid
C22:6 Docosahexaenoic acid
12 FAMEs AGILENT TECHNOLOGIES APPLICATION NOTEBOOK
RESULTS AND DISCUSSION

25
Figure 2 shows the separation of FAMEs from salmon oil on an Agilent 7696A
Mean 23, 42%
WorkBench. The separation allows the unequivocal identification of all FAMEs. EPA %
22.5
The two compounds of main interest show retention times of 35.07 minutes
(EPA) and 40.55 minutes (DHA). Besides EPA (23.7%) and DHA (20.0%),
20
salmon oil further consists of unsaturated fatty acids oleic (12%), linoic (11%) Mean 18, 85%
and palmitoleic (8%) acid. The content of saturated fatty acids, palmitic and DHA %
17.5
stearic acid, is low, 4% and 5%, respectively.
For the repeatability test, 10 individual salmon oil samples were derivatized 15
0 2 4 6 8 10
and analyzed to determinate the reproducibility of the automatic sample Sample number
preparation and chromatography. As shown in Figure 3, excellent repeatability Figure 3. Repeatability data of of automated FAME determination in salmon oil
was obtained. The absolute areas of the EPA and DHA signals showed standard
deviations of less than 1% (EPA 0.51%, DHA 0.78%). Moreover, variations CH3 O CH3
of the EPA and DHA relative concentrations were stable. Relative standard O
deviations of 0.85% for EPA and 1.22% for DHA were achieved. No outliers O
were observed over the 10 samples. H3C O CH3
The total runtime for sample preparation on the Agilent 7696A Sample Prep
WorkBench was only 20 minutes per sample, whereas the time for the manual
derivatization depends on the skills of the laboratory technician and can take Figure 4. Structure of EPA methyl ester (left) and DHA methyl ester (right)
up to 2 hours.
pA
35.066
400
C20:5
25.944
EPA
350
24.200
C18:2
300
C18:1
40.550
250 C16:1
C16:0 C18:3
19.976
200 C20:1
C22:1
18.796
C20:0 C20:4
150 C18:0 C22:6
C24:1 DHA
29.250
C14:0
27.870
100
22.961
32.706
28.168
C18:3
33.975
15.927
27.062
50
37.011
0
15 20 25 30 35 40 min
Figure 2. GC/FID chromatogram of a salmon oil sample, prepared using Agilent WorkBench 7696A
Table 2. Percent distribution of fatty acids in salmon oil sample

C14:0 C16:0 C16:1 C18:0 C18:1 C18:2 C20:0 C18:3 C20:1 C18:3 C22:1 C20:4 C20:5 C24:1 C22:6
0.71 4.68 7.95 3.54 12.95 13.86 0.36 2.61 1.71 3.33 3.35 0.87 23.79 0.36 19.93
AGILENT TECHNOLOGIES APPLICATION NOTEBOOK FAMEs 13
CONCLUSION
The automated sample derivatization is easy, fast, and reliable. For samples
with high relative concentrations of polyunsaturated fatty acids especially, the
automation is significantly more reliable than manual procedures.
REFERENCE
(1) Animal and vegetable fats and oils – Gas chromatography of fatty acid methyl
esters – Part 3: Preparation of methyl esters using trimethylsulfonium hydrox-
ide (TMSH) (ISO 12966-3:2009)

Published in USA
14 Marine Toxins AGILENT TECHNOLOGIES APPLICATION NOTEBOOK
Method for the Determination of Chemical Contaminants

in Marine Shellfish
Agilent Technologies, Inc.
INTRODUCTION KEY BENEFITS

Chemical contaminants that are released into the marine environment may • Sample extraction based on a modified QuEChERS method
be ingested (absorbed) by fish and shellfish and thus become introduced • Recoveries for all analytes in the range of 85.4% to 123.9%
into the human food chain. Lipophillic chemicals such as OCPs and PCBs can • Large-volume (solvent vent mode) injection using a multimode inlet
bioaccumulate in the fatty tissues of marine fish and shellfish. The longer an ensuring required detection limits are met
organism is exposed to a contaminated environment, the higher the likely • Retention time locked chromatographic method for ease of set-up and
levels of contaminants. on-going maintenance
The Clean Seas Environmental Monitoring Program (CSEMP) is an initiative • Capillary flow technology for post-column, post-run backflush to ensure
designed to monitor the levels of chemical contamination in the United chromatographic method robustness and prevent contamination of the
Kingdom’s coastal and estuarine areas. The major drivers for this program are: MS ion source with high-boiling matrix
• To meet the mandatory monitoring requirements under Oslo and Paris • Mass Hunter software that is very powerful yet easy to master, providing
Convention (OSPAR) Joint Assessment and Monitoring Program (JAMP) excellent data review capabilities and easy, flexible reporting.
• To comply with EC Directives.
Agilent Technologies has partnered with a leading European Analytical
Laboratory to develop a sample preparation method based on a modified
QuEChERS extraction along with a GC/MS/MS method for the determination
of selected OCPs, PAHs, and PCBs in marine shellfish (Mussel) tissue. The GC/
MS/MS method provides reproducible and sensitive determination of OCPs,
PCBs, and PAHs that employs large-volume (solvent vent) injection using a
Multimode inlet (MMI) and post-column, post-run backflush in order to remove
high-boiling matrix components that would otherwise remain in the column
between analyses and subsequently cause degradation of chromatographic
performance and contamination of the mass spectrometer ion source.
The analytical method meets the detection limit requirements of 0.1 μg/Kg for
OCPs and PCBs, and 0.5–1.0 μg/Kg for PAHs.
Figure 2. MRM chromatograms for (I) incurred a-HCH and (II) incurred g-HCH in
COMPOUNDS mussel sample, concentrations 0.06 and 0.30 μg/Kg, respectively. Peaks (III)
• 16 OCPs and (IV) are traces of incurred b-HCH and d-HCH, respectively
• 19 PAHs
• 7 PCBs
Figure 1. TIC MRM chromatogram of a calibration standard mixture of OCPs, PAHs and PCBs*
www.agilent.com/chem Figure 3. MRM chromatograms for (I) incurred fluoranthene and (II) incurred pyrene
Agilent shall not be liable for errors contained herein or for incidental or consequential damages in connection in mussel sample, Concentrations 8.64 and 5.83 μg/Kg, respectively
publication are subject to change without notice. * Full analytical details are available in Agilent Technologies publication 5990-7714EN.

Published in USA
AGILENT TECHNOLOGIES APPLICATION NOTEBOOK Flavors 15
Analysis of Medium Volatility Sulfur Compounds

in Coffee Using Agilent GC/Q-TOF
INTRODUCTION ×107
1.05
The resolution, sensitivity, and mass accuracy of the Agilent 7200 GC/Q-TOF 0.95
system provide rapid, simple, and reliable analysis of trace levels of sulfur 0.85
0.75
compounds in coffee. 0.65
0.55
Volatile sulfur, containing compounds present in coffee, plays an important 0.45
0.35
role in aroma and flavor. Characterization of desirable coffee aroma can 0.25
be a challenging task, since many of these compounds are present in trace 0.15
0.05
amounts. Identification and quantitation of sulfur compounds present in 6.0 6.5 7.0 7.5 8.0 8.5 9.0 9.5 10.0 10.5 11.0 11.5 12.0 12.5 13.0 13.5 14.0 14.5 15.0 15.5 16.0 16.5 17.0 17.5 18.0
Counts versus acquisition time (min)
complex food matrices at trace levels (low ng/mL in matrix) often requires Figure 1. TIC of coffee extract (not spiked with sulfur compound standards),
time-consuming sample preparation as well as elaborate techniques with illustrating the complexity ot the matrix
high separation power, such as 2D GC combined with mass spectrometry. ×104
×104
Using the resolution, sensitivity, and speed of an Agilent GC/Q-TOF system, 1.5 110.9899 2-Formyl Thiophene, EIC
consistent product quality can be monitored with minimal sample preparation 2
80.0496
93.0448 m/z 111.9977 +/- 10 ppm
4.5 ng/mL
and a standard 1D GC method. 1
81.0572
94.0547 111.9974
1
107.0604
For the GC/Q-TOF method, a simple liquid-liquid extraction is adequate 0.5
sample preparation before the analysis of medium volatility sulfur compounds
0
80 85 90 95 100 105 110
Counts vs. Mass-to-Charge (m/z)
in coffee. High-resolution mass spectra with low mass error help to resolve 0
4.5 5 5.5 6 6.5 7 7.5 8 8.5
compounds of interest from severe matrix interferences. The 7200 GC/Q-TOF Counts vs. Acquisition Time (min)
provides low pg method detection limits with less than 5 ppm error in mass ×103
accuracy. Linearity up to three orders of magnitude in matrix is achieved with 2
×104
1 2-Acetyl Thiazole, EIC
99.0137
a correlation coefficient > 0.995. Standard addition method was successfully m/z 127.0086 +/- 10 ppm
2 ng/mL
applied for determination of 2-formyl thiophene and 2-acetyl thiazole 0.5
concentrations at ng/mL levels naturally occurring in coffee extract. 1

57.9867 68.9936 83.9903
111.9856 127.0080
In summary, an Agilent 7200 GC/Q-TOF system is able to provide trace-level

0
50 60 70 80 90 100 110 120 130
Counts vs. Mass-to-Charge (m/z)
compound profiling in complex food matrices, without the need for complex 0
4.5 5 5.5 6 6.5 7 7.5 8 8.5
and tedious sample preparation and separation methods. Counts vs. Acquisition Time (min)
The method was developed by Nobuo Ochiai and Kikuo Sasamoto of Gerstel Figure 2. EIC and mass spectra of 2-formyl thiophene and 2-acetyl thiazone at their
K.K. and Ryo Ogasawara and Sofia Aronova of Agilent Technologies, Inc. natural levels extracted from a coffee matrix
KEY BENEFITS
• The Agilent 7200 GC/Q-TOF enables a fast and simple method for routine Table 1. Mass error for 2-formyl thiophene and 2-acetyl thiazole
analysis of sulfur compounds in complex food matrices. measured in spiked coffee extract
• High sensitivity allows qualitative and quantitative analysis of volatile sulfur Mass error, ppm
compounds in coffee down to 1 pg on column. pg on column 2-formyl thiophene 2-acetyl thiazole
• The resolution and mass accuracy of the Agilent 7200 Series GC/Q-TOF 1 -3.57150 -0.78735
provide sufficient selectivity for analyte quantitation in complex food 2 -4.46438 -0.78735
5 -2.67863 -0.78735
matrices. 10 -2.67863 0.78735
• Linearity up to three orders of magnitude facilitates quantitation over a 20 -2.67863 0.00000
50 -0.89288 1.57470
large concentration range. 100 0.00000 1.57470
200 -1.78575 1.57470
500 2.67863 -1.57470
1000 1.78575 -1.57470
Average 2.32148 1.10229

Published in USA
Simple, Rapid Analysis of Trace Metals in Foods

Using the Agilent 7700x ICP-MS
Steve Wilbur Agilent Technologies, Inc. Everett, Washington Michiko Yamanaka, Agilent Technologies Tokyo Analytical Division, Tokyo, Japan
INTRODUCTION Table 2. List of analytes and acquisition times (All elements were
The task of efficiently monitoring chemical and biological contaminants in acquired in He mode)
imported and exported food can be overwhelming. Traditionally, analysis Integration time
of metals in foods has required multiple techniques in order to cover the Mass Element per mass (sec) Replicates
range of elements, concentrations, and food types. This approach is slow 6 Li 0.3 3 Internal standard
and expensive, so a more rapid, sensitive, and cost-effective screening test 9 Be 0.99 3
is necessary. The Agilent 7700x ICP-MS is capable of accurately analyzing a
23 Na 0.3 3
variety of foods for metals at trace and major levels using a single collision
40 Ca 0.3 3
cell method. This method is simple to set up and operate routinely, and
permits large numbers of samples to be quickly screened for total toxic 43 Ca 0.3 3
metals. Samples that are found to contain metals where the potential 45 Sc 0.3 3 Internal standard
toxicity is dependent on the chemical form can then be further analyzed for 51 V 0.3 3
species composition as needed, using Agilent-supported hyphenated ICP-MS 52- 53 Cr 0.3 3
techniques such as LC-ICP-MS or GC-ICP-MS. 55 Mn 0.3 3
EXPERIMENTAL 56 Fe 0.3 3
To test the ability of the Agilent 7700x to analyze a variety of foods for a wide 60 Ni 0.99 3
range of metals at highly variable concentrations, several certified reference 63 Cu 0.3 3
food samples were analyzed. The 7700x was tuned using One-Click Plasma 66 Zn 0.3 3
setting for robust plasma conditions and autotuned for optimum sensitivity, 72-74 Ge 0.3 3 Internal standard
mass response, and minimal interferences. Operating conditions are shown 75 As 0.99 3
in Table 1. To keep the method as quick and simple as possible, the Octopole
77-78, 82 Se 0.99 3
Reaction System (ORS3) was operated in a single mode, using helium (He)
95 Mo 0.99 3
cell gas, which provides a reliable and effective cell method to remove all
polyatomic interferences, regardless of the analyte or matrix composition. 111 Cd 0.3 3
The following acquisition masses and integration times (Table 2) provided 115 In 0.3 3 Internal standard
more than sufficient sensitivity to meet all certified values. Total run time per 121 Sb 0.99 3
sample was less than 3 minutes. 137 Ba 0.3 3
Table 1. 7700 Autotuning Conditions 159 Tb 0.3 3 Internal standard
Parameter Value 202 Hg 0.99 3
205 Tl 0.99 3
Set by One-Click RF power (W) 1550
208 Pb 0.3 3
Plasma Setting Carrier gas flow (L/min) 0.99
209 Bi 0.3 3 Internal standard
Spray chamber temp (°C) 2
238 U 0.99 3
Sample depth (mm) 8
Extract 1 lens (V) 0
Set by Autotune CeO+/Ce+ (%) 1.114

Ce++/Ce+ (%) 1.867
Sensitivity cps/ppb Li (62700), Y (92920),
Tl (87080)
Traditionally, covering this range of concentrations for these elements would

have required ICP-OES for the major elements (Na and Ca), graphite furnace
AA for Pb and Cd, either a dedicated Hg analyzer or cold vapor AA for Hg and
possibly hydride AA for As and Se. The Agilent 7700x ICP-MS running in He
mode was able to measure all elements in a single run easily. Even elements
such as Be and Hg, which would typically be acquired under no-gas conditions
when using ICP-MS, demonstrated excellent sensitivity in He mode (Be DL =
28 ppt, Hg DL = 1.6 ppt).
Example calibration curves for several critical and difficult elements are shown in Figure 1.
Figure 1. Calibrations for Be, Cr, As, Se, Cd, and Hg.
ATTAIN
SUPERIOR
MASS SPEC PERFORMANCE
Confidence means attaining superior analytical performance, attaining
24/7 reliability, maximum uptime and productivity—everything you
expect from the leader in mass spectrometry. Across your MS platforms,
Agilent provides one single, consistent user interface. After 40+ years of
innovation and expansive experience with the industry’s largest installed
base, Agilent’s best-in-class portfolio continues to push the boundaries
of MS technology, delivering market-leading solutions.
Learn more about Agilent Mass Spec technology at
www.agilent.com/chem/MSPerformance
Scan the QR code for more information

about Agilent’s LC/MS, GC/MS, ICP-MS
and MassHunter Software

CONCLUSIONS
The food certified reference materials were analyzed directly after microwave Using a simple procedure based on microwave digestion and single He mode
digestion. Between 0.5 g and 1 g of each sample was weighed (after determination ICP-MS analysis, typical food samples can be quickly and accurately analyzed
of percent moisture) and digested using 6 mL of HNO3 + 2 mL of H2O2 using for trace and major element concentrations without the need for multiple
microwave assisted digestion. All samples were brought to final volume of sample preparations and analytical techniques. The Agilent 7700x using He
100 mL using ultrapure water. Results are shown in Table 3. The trace elements, mode alone can provide sensitive, accurate, interference-free analysis of a
Ni, Mn, Cu, As, Se, Cd, Hg, and Pb exhibited excellent agreement with the variety of metals in common foods. Because He mode is both sensitive and
certified values for all three samples. Slight deviations from certified values universal, it is applicable to trace analysis of all metals in any food sample
for Fe, Ca, and Zn were attributed to the digestion procedure rather than the digest. No prior information about the sample matrix or analyte elements
analytical measurement. present is required, as He mode removes all polyatomic interferences,
regardless of the sample matrix.
Table 3. Measured and certified values for three certified reference food materials. Recoveries are dependent on digestion efficiency as
well as analytical accuracy. All measured values are based on dry sample weight corrected for percent moisture. All certified
elements are reported for each sample; not all samples are certified for all elements
NRC-CNRC DORM3 NIST SRM 2976 NIST RM 8415

Fish protein Mussel tissue Whole egg powder
Certified value Measured Certified value Measured Certified value Measured

Mass/element (mg/kg) (mg/kg) (mg/kg) (mg/kg) (mg/kg) (mg/kg)
23 Na – – – – 3770 ± 340 3807

43 Ca – – – – 2480 ± 190 2703
52 Cr – – – – 0.37 ± 0.18 0.344
55 Mn – – – – 1.78 ± 0.38 1.64
56 Fe 347 ± 20 324.0 171 ± 4.9 158.5 – –
60 Ni 1.28 ± 0.24 1.29 – – – –
63 Cu 15.5 ± 0.63 14.4 4.02 ± 0.33 3.32 2.7 ± 0.35 2.61
66 Zn 51.3 ± 3.1 45.86 137 ± 13 121.2 – –
75 As 6.88 ± 0.3 6.15 13.3 ± 1.8 12.57 – –
78 Se – – 1.8 ± 0.15 1.87 1.39 ± 0.17 1.25
95 Mo – – – – 0.247 ± 0.023 0.215
111 Cd 0.29 ± 0.02 0.28 0.82 ± 0.16 0.794 – –
202 Hg 0.355 ± 0.056 0.359 0.061 ± 0.0036 0.068 – –
208 Pb 0.395 ± 0.050 0.398 1.19 ± 0.18 1.163 0.061 ± 0.012 0.055

Published in USA
20 Dioxins AGILENT TECHNOLOGIES APPLICATION NOTEBOOK
A Reliable and Routine GC/MS/MS

Method for the Determination of Dioxins in
Foodstuffs and Animal Feed
ASSURE Agilent Technologies, Inc.

INTRODUCTION
FOOD SAFETY
Polychlorinated dibenzo-p-dioxins (PCDD) and polychlorinated dibenzofurans (PCDF) are fat-soluble,
highly toxic, ubiquitous environmental contaminants found at trace levels in all foodstuffs and animal
ANALYSIS
feed. Current legislation in the European Union (EU) and the United States requires the confirmation
of PCDD and PCDF congeners by GC-high resolution mass spectrometry (GC-HRMS). In the event of a
food-related dioxin contamination incident, many samples must be analyzed in as short a time as possible
Confidence means having the in order to determine the extent of the contamination and the subsequent potential risk to human health.
best tools at every stage of your Agilent Technologies has partnered with a leading European dioxin laboratory to develop a method based
food analysis to assure accurate on GC/MS/MS for the trace analysis of PCDD and PCDF congeners in foodstuffs and animal feed. The
and reproducible results. Elevate method provides sensitive and reproducible results that are comparable to those obtained by GC-HRMS.
confidence in food safety with The GC/MS/MS method meets the requirements of current EU legislation for the screening of PCDD
Agilent J&W Ultra Inert GC and PCDF congeners in foodstuffs and animal feed, and has potential as an alternative confirmatory
columns, fast LC and advanced methodology for the determination of PCDD and PCDF congeners in official food and feed control,
sample preparation products for pending analytical quality criteria to be set by legislative bodies.
complex food matrices.
COMPOUNDS
• As specified in US and EU legislation
• 7 PCDD congeners
• 10 PCDF congeners
KEY BENEFITS
• Retention-time locked method for ease of chromatographic set-up.
• Capillary flow technology provides concurrent backflush for improved method robustness.
• Excellent linearity and response reproducibility for dioxins in foodstuffs and animal feed over the
range of interest.
• Reproducible response even at low fg levels on column.
• Detection down to low pg WHO-TEQ/g.
• Chromatographic results that meet legislated screening requirements for EU methods.
• Mass Hunter software that is very powerful yet easy to master, providing excellent data review
capabilities and easy, flexible reporting of data.
To learn more about Agilent sample

prep, and LC and GC columns
solutions for food safety, visit:
www.agilent.com/chem/assure

AGILENT TECHNOLOGIES APPLICATION NOTEBOOK Dioxins 21
BOOST
FOOD ANALYSIS
RELIABILITY
Confidence means avoiding false
positives and negatives in your
analysis without sacrificing scan
speed or sensitivity. Boost the
Figure 1. Chromatographic separation of native PCDD and PCDF congeners* reliability of your food safety
testing with triggered MRM. Use
an Agilent Triple Quadrupole Mass
* Full analytical details are available in Agilent Technologies publication 5990-6594EN.
Spectrometer to simultaneously
quantify and confirm contaminants
Figure 2. Relative difference in the sum of PCDD/PCDF congener quantitative results (TEQ WHO98 in difficult matrices.
upperbound values) for 40 foodstuff and animal feed samples analyzed by GC-HRMS and
GC/MS/MS
To learn more about LC/MS and

tMRM methods in food safety, visit:
www.agilent.com/chem/tMRM_food
Published in USA
22 Wine Profiling AGILENT TECHNOLOGIES APPLICATION NOTEBOOK
A Prediction Model for Determining Wine

Variety Using the Agilent LC/MS Q-TOF
and Agilent
ENSURE This work was reported in L. Vaclavik, O. Lacina, J. Hajslova, J. Zweigenbaum, Analytica Chimica
Acta 2011, 685, 45 (http://www.sciencedirect.com/science/article/B6TF4-1GHWXP-1/2/
e70f1f1928475f12c9341d8b67e05310).
FOOD SAFETY
DATA INTEGRITY INTRODUCTION
Wine is a beverage produced and consumed throughout the world and is a highly valued commodity.
Confidence means ensuring accuracy Its classification and authenticity can be very important. The constituents of wine are complex and
and integrity of your analytical data include compounds that impart taste, color, and other characteristics that determine the quality of the
in heavily regulated environments. beverage. One component is the type of grape used and the question this study examines is whether
Agilent OpenLAB Enterprise Content there are specific compounds in wine that distinguish one grape from another. Using wines obtained
Manager (ECM) and Agilent OpenLAB from around the world, the power of accurate mass and high resolution is put to use by analyzing three
Electronic Lab Notebook (ELN) help varieties of wine: Pinot Noir, Merlot, and Cabernet Sauvignon. Using Agilent’s Mass Profiler Professional
ensure compliance. With Agilent’s software, the resulting single MS data containing over 26000 entities are statistically evaluated. Once
open informatics suite you can filtered on differences, principle component analysis shows that the wine variety can be grouped by
capture, analyze, and share vital specific compounds found in the wine samples. With this knowledge, a model based on partial least
information–from any instrument, squares differentiation is made and unknown wines can be classified. All this is done without knowing
in any data format. the identity of the marker compounds that can distinguish one grape from another.
Try OpenLAB ELN for free: Using the Agilent 6530 Accutate-Mass Q-TOF LC/MS, MS/MS can be performed on the ions shown to
www.agilent.com/chem/openlabFREE correlate specific grapes, and identification can be pursued with the excellent accurate mass measurements.
It is noted that the identification of true unknowns, compounds not found in any database, is a difficult task.
However, identification is not necessary for this type of determination and even the unidentified compounds
can be used with their MS/MS signatures for routine classification. This study demonstrates the power
of the Agilent LC/MS Q-TOF in combination with Mass Profiler Professional’s multivariate statistical
capabilities designed specifically for MS data processing.
KEY BENEFITS
• Agilent 6500 Series Q-TOF LC/MS provides the sensitivity, mass accuracy and resolution needed to
separate unique compounds recognizing a wine’s variety.
• Mass Profiler Professional provides the needed multivariate statistics directly on accurate mass
spectral data.
• Mass Profiler Professional provides powerful models for prediction analysis.
• Comprehensive workflow wizards guide the experimenter through statistical analysis of their data to
obtain powerful correlations and visualization of the results.
• With Q-TOF MS/MS, the identity of marker compounds may be obtained.
To learn about OpenLAB Informatics

Suite in food safety, visit:
www.agilent.com/chem/ensure

AGILENT TECHNOLOGIES APPLICATION NOTEBOOK Wine Profiling 23
AFFIRM
FOOD SAFETY
STANDARDS
Confidence means affirming your
instruments are globally certified
to maintain the strictest food
Figure 1. Total Ion Chromatogram on wine sample injected directly shows the complexity of the data
safety standards. Affirm your
proof-of-system maintenance and
calibration with Agilent’s Functional
Verification Services. Standardize
maintenance protocols and validate
testing methodology across all your
chromatography systems worldwide.
Figure 2. Principal component analysis of filtered results shows that Merlot, Cabernet Savagnoun, and
Pinot Noir wines can be distinguished by these marker compounds.
To reduce regulatory risk and

streamline ISO 17025 documentation/
certification process, visit:
www.agilent.com/chem/FVSfood
Published in USA
SIMULTANEOUS ANALYSIS OF HUNDREDS OF PESTICIDES IN FOOD
SAMPLES USING THE AGILENT 6400 SERIES TRIPLE QUADRUPOLE LC/MS
The Challenge
More than 1000 pesticides are currently used worldwide in the treatment of soil systems utilize the UHPLC columns to provide very fast separations (<20 minutes)
and crops. Many countries have established allowable levels of those pesticides in and very sharp peaks for the 300 pesticide method that maximize the number of
food to protect consumers. While these maximum residue levels (MRLs) vary, the components that can be identified and quantified (Figure 1).
default tolerance is 10 parts per billion (ppb). However, the MRL for pesticides in
baby food can be as low as 4 ppb.
These pesticides have to be monitored as part of the quality control of food,
especially fruits and vegetables, challenging food producers to detect and quantify
hundreds of compounds present at minute levels. Since analyzing all of these
compounds separately is not feasible, multi-compound methods are required.
However, the ability to monitor hundreds of pesticides at once is a challenging
problem for chromatography and mass spectrometry.
Meeting the Challenge

A method that can simultaneously detect and quantify hundreds of pesticides
requires a liquid chromatography (LC) system that can generate very sharp peaks
and rapid separations. It also requires a triple quadrupole mass spectrometer (MS)
that can provide excellent selectivity and sensitivity in very complex matrices,
along with short dwell times that allow the analysis of peaks only seconds in width.
Rapid and effective development of multi-pesticide methods also requires a Figure 2. The number of compounds detected in extracts of a variety of fruits and
reliable and fast sample extraction method, as well as access to a database that vegetables spiked with the 300 pesticide mix at concentrations from 0.1 to 100
ppb, using the 1290 Infinity UHPLC and the 6490 Triple Quadrupole LC/MS.
contains method parameters for hundreds of compounds.
The Agilent Solution The Agilent 6400 series Triple Quadrupole LC/MS systems are also used with
the kit to provide fast, multi-analyte quantification. They utilize Dynamic MRM,
Development of methods that can screen and quantify hundreds of pesticides can
which monitors analytes only when they are eluting from the LC, to shorten cycle
be a daunting task. Agilent provides an effective solution that addresses all of the
times and maximize the number of compounds detected in a chromatogram
key requirements for successful method development. The Pesticides Dynamic
without dividing it into segments. The Jet Stream and Ion Funnel technologies also
MRM Database Application Kit includes a database with conditions, transitions
available with the 6400 series provide the sensitivity to detect as low as sub-ppb
and retention times for more than 750 compounds that can be used to generate
levels of pesticides in a wide range of fruit and vegetable matrices. (Figure 2).
custom methods. In addition, a pre-configured method for 300 pesticides is
included with the kit. For more details on the Pesticides Dynamic MRM Database Application Kit, 1200
Infinity Series LC systems, and 6400 Series Triple Quadrupole LC/MS systems for
We recommend Bond Elut QuECheRS extraction and dispersive kits for optimal
pesticide applications, visit the Agilent Technologies web site at: www.agilent.com.
sample prep. A ZORBAX Eclipse Plus UHPLC column provides excellent resolution
on short columns for high sensitivity and rapid separations. The 1200 series LC
×10 6 1 13.9 1
11.9
1
12.1
0.9 10.7
14.8
0.8 8.5
0.7
9.5
0.6 8.7
9.8 13.0
0.5 11.5
10.5
5.7 9.1
0.4 12.7
6.0
10.1
4.3
0.3 7.0 7.3
2.8
5.2
15.3
Figure 1. Extracted Ion Chromatogram (EIC) of a 300-compound
0.2 3.8 5.4
2.5 6.3 14.4
8.2
0.1
3.2
4.0
6.7
pesticide mixture using the Agilent 1290 Infinity UHPLC.
7.5
The retention time is shown above each peak.
1.8 2.4
0.7 1.0 1.4 4.8 16.1 17.5
1 2 3 4 5 6 7 8 9 10 11 12 13 14 15 16 17
Counts vs. acquisition time (min)
AGILENT TECHNOLOGIES APPLICATION NOTEBOOK Mycotoxins 25
Triple Quadrupole LC/MS Analysis of Aflatoxins

in Various Food Samples
INTRODUCTION
Triple quadrupole LC/MS analysis of aflatoxins in food samples eliminates
The Agilent LC/MS/MS provides the necessary limits of reporting for aflatoxins
the need for expensive immuno-affinity cleanup columns and reduces the
and reduces false positives and negatives to the lowest levels of probability. This
probability of false positives to almost zero.
provides the assurance needed for a safe food supply. With DSPE for sample
Aflatoxins are highly carcinogenic secondary metabolites of the molds preparation, the day-to-day method is cost-effective and efficient.
aspergillus flavus and aspergillus parasiticus and are found in grains, corn,
KEY BENEFITS
peanuts, and other foodstuffs. The action level for these toxic naturally
• Agilent 6460 Triple Quadrupole LC/MS provides high sensitivity for
occurring compounds is typically 20 ppb around the world for food and animal
carcinogenic aflatoxins with limits of detection (LODs) well below action
feed. Japan has a more aggressive limit of 10 ppb for Aflatoxin B1 and is now
levels in food and feed.
changing that to 10 ppb total aflatoxin. This method uses the highly selective
and sensitive triple quadrupole LC/MS/MS in Multiple Reaction Monitoring • The highly selective LC/MS/MS requires less expensive sample preparation.
(MRM) mode and can achieve sensitivities in food matrices that are well below • Quantitation and confirmation are performed in one analysis.
these action levels. In addition, the expensive immuno-affinity solid phase • More samples can be analyzed and reported faster.
extraction (SPE) is compared, in this limited study, to the very inexpensive
• Agilent provides everything needed from dispersive SPE material to
dispersive solid phase extraction (DSPE) and found to be equivalent.
columns and supplies.
The method was developed with the Agilent 6460 Triple Quadrupole LC/
MS with focusing Agilent Jet Stream Technology and the Agilent 1200
Series LC including the Agilent 1260 Infinity Binary Pump and the 1200
Series High Performance Well Plate Sampler SL Plus. This high-performance
method achieves near baseline separation of each of the four compounds
in less than 5 minutes. In addition, the method uses three transition ions:
one for quantitation and two for qualifiers providing sensitive and accurate
quantitation and confirmation by comparing ion ratios and retention times to
standards. This eliminates false positives and the need for further analysis to
obtain confirmation. The use of stable isotope internal standards added to the
samples prior to extraction provides correction for any matrix affects in both
extraction and analysis, and assures near zero probability of false negatives.
Figure 1. LC/MS/MS chromatogram of aflatoxin B1, B2, G1, and G2 standards at 1 ppb
Food B1 B2 G1 G2
matrix LOD (ng/g) LOD (ng/g) LOD (ng/g) LOD (ng/g)
Corn 0.060 0.085 0.100 0.033
Wheat 0.012 0.037 0.150 0.110
Peanut 0.056 0.069 0.050 0.140
Walnut 0.093 0.098 0.120 0.040
Average 0.055 0.072 0.105 0.080
Mass On-Column 275 fg 360 fg 525 fg 400 fg
Figure 2. LOD results observed for Aflatoxins B1, B2, G1, and G2 with dispersive SPE sample preparation

Published in USA
Identification and Quantitation of Pesticides in Chamomile and

Ginger Extracts Using an Agilent 6460 Triple Quadrupole LC/MS
System with Triggered MRM
Thomas Glauner, Agilent Technologies, Inc., Waldbronn, Germany Tiffany Payne, Agilent Technologies, Inc., Santa Clara, CA USA Guenther Kempe,
Stefan Kittlaus, Daniela Goermer, State Laboratory for Health and Veterinary Affairs Saxonia, Pesticide Department, Dresden, Germany
ABSTRACT MRM transitions in a similar ratio. Tebufenpyrad co-elutes with an endogenous

This application note describes the use of triggered Multiple Reaction ginger compound that shares the same primary MRM transitions. For both
Monitoring (tMRM) for the analysis of pesticide residues applied to chamomile analytes in a conventional MRM analysis, the endogenous compounds in
and ginger extracts. The analysis is performed using the Agilent 1290 LC the matrix may result in a false positive result. However, tMRM analysis was
system coupled to a 6460 Triple Quadrupole LC/MS with tMRM acquisition. able to differentiate the endogenous compound in ginger from tebufenpyrad
Two examples of false positive identifications were explored: tebuthiuron in contamination using eight additional product ions for the observed
chamomile and tebufenpyrad in ginger. Both compounds were quantitated contaminant to perform library confirmation. In addition to the retention time
and confirmed with library matching in a single analytical run. False positive for tebuthiuron, which can be influenced by the sample matrix, tMRM analysis
identification was avoided by using library matching and tMRM acquisition. allowed the unambiguous identification of tebuthiuron offering an enhanced
level of confirmation. The power of tMRM acquistion comes from its ability to
INTRODUCTION
provide quantitative and qualitative data in a single analytical injection.
Modern multiresidue methods for pesticide analysis typically cover hundreds
of compounds of different chemical classes. This same method is also typically The tMRM analysis starts with a MRM scan of the designated primary MRM
applied to different matrices. Commonly, this type of analysis is performed transitions for each compound, covering a range of possible target analytes.
using a fast-scanning instrument—usually a triple quadrupole—which is set When the signal for a given primary transition reaches a user-defined threshold,
up to acquire two MRM transitions (one quantitative and one confirmatory the secondary transitions are triggered automatically. Each compound is
transition) for each of the chosen analytes. allowed a total of 10 MRM transitions in tMRM mode. These 10 transitions
include the primary and secondary MRM transitions in any combination
In Europe, the analysis of pesticides in food products is based on commission
(one primary and nine secondary MRMs, two primary and eight secondary,
regulation (EC) No. 396/20051 and its annexes, which specify the
etc). This type of acquisition maximizes the dwell time for all possible target
maximum residue limits for pesticides in different products. As of March
analytes in the primary MRM screening phase, and then acquires sufficient
11, 2008, there are maximum residue limits (MRLs) defined for more than
MRM data for the detected analytes to compose a product ion spectrum. The
170,000 matrix-pesticide combinations by the European Union. Guideline
generated product ion spectra can be used for library searching, so that at
SANCO/10684/20092 sets criteria for method validation and quality control
the end of the tMRM analysis rigorous quantitative data and a product ion
procedures for pesticide residue analysis in food and feed. For LC/MS triple
spectrum with the accompanying confirmatory library match are acquired. By
quadrupole analysis, the identification criteria include retention time, m/z
applying the optimized collision energy and dwell time for each product ion,
value, and abundance data. In addition, the retention time of the analytes
tMRM is significantly more sensitive than conventional product ion scanning.
must not vary beyond 2.5%. Multiple reaction monitoring with two or more
product ions and a constant ion ratio have specified tolerances of ±20% to EXPERIMENTAL
50% depending on their relative intensity to the base peak. Sample Preparation
Samples have been prepared according to §64 LFGB QuEChERS3 without
For this work, 51 pesticides were analyzed using tMRM acquisition with
modification. Ten grams of homogenized ginger sample were extracted with
an Agilent 6460 triple quadrupole LC/MS. We examined two pesticides in
10 mL of acetonitrile. For the chamomile extract, the sample amount was
particular for which there have been reports of false positives in the past:
reduced to 2 g and samples were diluted with 10 mL water before extraction.
tebuthiuron (a broad-spectrum herbicide recently reported for a chamomile
MgSO4, NaCl, and sodium citrate were added and then centrifuged for 5
sample) and tebufenpyrad (a pyrazole acaricide and insecticide reported
minutes at 3000 rpm. Clean-up was performed by dispersive SPE. Six mL of
falsely for ginger). These two pesticides exemplify two common analytical
the supernatant was transferred to a d-SPE tube with 900 mg MgSO4 and
scenarios under the applied method conditions. Tebuthiuron is well-resolved
150 mg PSA. For the chamomile sample, 45 mg of graphitized carbon black
from the neighboring endogenous matrix interference showing both primary
was also added. After centrifugation, 5 ml of the supernatant were stabilized
with 50 µL of 5% formic acid in acetonitrile.
Table 1. LC Conditions LC/MS ANALYSIS

Instrumentation
LC column ZORBAX Eclipse Plus C-18 RRHD column 100
x 2.1 mm, 1.8 µm @ 30 °C The Agilent 1290 Infinity LC system is coupled to an Agilent 6460 triple
quadrupole LC/MS.
Mobile phase A = 5 mM ammonium formate in water
B = 5 mM ammonium formate in methanol LC CONDITIONS
Gradient program 5% B for 0.2 minutes; ramp up to 30% B Table 1 shows the LC parameters used for analysis of pesticides in ginger and
over 2 minutes; ramp up to 100% B over 8.3 chamomile extracts using tMRM acquisition.
minutes; hold for 2.5 minutes; bring to 5% B;
hold for 2 minutes MS CONDITIONS
Flowrate 0.500 mL/min
Table 2 shows the MS parameters used for the analysis.
Injection volume 2 µL RESULTS AND DISCUSSION

This LC/MS method separated and detected 51 pesticides. Although the
tMRM experiment allowed a total of 10 MRM transitions per compound,
Table 2. MS Conditions the compounds in this analysis utilized two primary transitions and up
to seven secondary transitions per compound. Figure 1 shows the overall
Ionization mode Agilent Jet Stream positive and negative mode Total Ion Chromatogram (TIC) and Extracted Ion Chromatogram (EIC) for a
API drying gas 7 L/min @ 200 °C quality control standard of all of the pesticides included in this method at the
API nebulizing gas 35 psi minimum reporting level (MRL).
Sheath gas 12 L/min @ 375 °C In order to acquire qualitative and quantitative information in a single analytical
Nozzle voltage +300/-500 V
run, tMRM acquisition was used.
Capillary voltage +3500/-3000 V

Cycle time 500 ms
Interscan delay 3.5 ms
Total number of MRMs 390
Maximum number of 84
concurrent MRMs
Minimum dwell time 3.64 ms
Maximum dwell time 146.5 ms
x105 A
1.4
1.2
1
0.8
0.6
0.4
0.2
0
1 2 3 4 5 6 7 8 9 10 11 12
Counts vs. Acquisition Time (min)
x104 B
7
6
5
4
3
2
1
0
1 2 3 4 5 6 7 8 9 10 11 12
Figure 1. Total Ion Chromatogram (A) and Extracted Ion Chromatogram (B) for 51 pesticides at the minimum reporting level (10 ng/mL)
The first analyte of interest was tebuthiuron in chamomile extract. Chamomile x104 x104
6.169 QC 50 ppb 1.5 6.365
contains an endogenous compound that shares the same mass and a similar 3
105934
RT 6.169 min
Blank Chamomile Extract 54241
RT 6.365 (+3.18%)
retention time to tebuthiuron. Figure 2 shows two chromatograms: the one on Qual/Quant ratio 22.5% 1 Calc.Conc. 12.6 µg/kg
Qual/Quant ratio
the left represents a tebuthiuron standard injection at 50 ppb and the one on 2
42.7% (189.9%)
the right represents an injection of a blank chamomile extract (one that was 1
0.5
known not to contain tebuthiuron). The data showed excellent peak shape and 0
0
signal for tebuthiuron, and that there are no co-eluting target analytes in our x105 x104
6.169 3.5 6.362
mix of 51 pesticide compounds of interest. Fortunately, the native compound 1.4 470039 3
126978
(although very similar in mass to charge ratio and retention time to tebuthiuron) 1.2
1
2.5
fell beyond the acceptable SANCO retention time variance guidelines for this 0.8
2
1.5
0.6
type of pesticide analysis, but still could be mistakenly identified as tebuthiuron. 0.4 1
0.2 0.5
The retention time for the native compound had a 3.18% difference from 0 0
5.9 6 6.1 6.2 6.3 6.4 6.5 6.6 5.9 6 6.1 6.2 6.3 6.4 6.5 6.6
the tebuthiuron standard (2.5% is the maximum deviation allowed), and Counts vs. Acquisition Time (min) Counts vs. Acquisition Time (min)
the qualifier-to-quantifier ion ratio was 189.9% of the expected ion ratio for
tebuthiuron. (The SANCO cutoff is 120% of the expected value.) Although the Figure 2. Primary MRM traces for tebuthiuron in 50 ppb quality control standard (left)
and in a blank chamomile extract (right). The top chromatograms represent
native chamomile extract compound in this case was similar to tebuthiuron, it the first qualifier traces for tebuthiuron (m/z 229.1 > 116.0) and the bottom
would likely be rejected as a match by applying the SANCO guidelines. In this chromatograms represent the quantifier traces (m/z 229.1 > 172.1)
case, tMRM analysis gave definitive proof that the endogenous compound
is not tebuthiuron, beyond the fact that the retention time for these two x106
compounds differed enough to force rejection by SANCO guidelines. 1 R2 = 0.9997
tMRM analysis was able to definitively identify the endogenous chamomile 0.9
compound by library matching. In addition, tMRM analysis was able to 0.8
qualitatively confirm that the endogenous chamomile compound was not 0.7
tebuthiuron. However, quantitative analysis was performed on tebuthiuron

Responses
0.6
spiked into a blank chamomile extract in order to demonstrate that in addition 0.5
to qualitative confirmation, tMRM acquisition is able to acquire reliable 0.4
quantitative data that one would expect from a high-performance triple 0.3
quadrupole mass spectrometer. Even though these compounds elute relatively 0.2
close to one another and triggered the acquisition of secondary transitions in 0.1
both cases, a blank chamomile extract spiked with tebuthiuron generated a 0
linear calibration curve with an R2 value equal to 0.9997 (Figure 3).

0 10 20 30 40 50 60 70 80 90 100
Five replicate injections of tebuthiuron at 10 ppb spiked into chamomile extract Concentration (ng/ml)
had a %RSD value of 0.94. Five replicate injections of the entire 51 pesticide Figure 3. Calibration curve for tebuthiuron in a blank chamomile extract from 1 ppb to
mix spiked into chamomile extract at 10 ppb had a %RSD value of 1.10. This 100 ppb. The R2 value for the calibration curve is 0.9997
method was found to produce linear and reproducible quantitative results.

In the case of tebufenpyrad in ginger extract, tMRM analysis was critical in x103
91.1 Acquired tMRM Spectrum
avoiding a false positive result for tebufenpyrad, even if SANCO guidelines 8 117.0 145.0 Native Ginger Compound
were applied. Figure 4 shows the chromatograms for the primary MRM 6
transitions for tebufenpyrad in a 50 ppb quality control standard (on the left)
versus an injection of a blank ginger extract that did not contain tebufenpyrad 4
(on the right). 2
In this case, the endogenous ginger compound (shown on the right in 334.2
0
Figure 4) varied only in retention time from the tebufenpyrad standard by x10 3
91.1
0.47% (well within regulatory guidelines). The qualifier-to-quantifier ion ratio 1 117.0 145.0 Comparison Acquired vs.
tMRM Library Spectrum
of the endogenous ginger compound was 123.1% of the expected ion ratio
for tebufenpyrad, and 120% is the regulatory cutoff set by SANCO guidelines.
334.2
This endogenous compound was very similar to tebufenpyrad and would 0
most likely give a false positive result using standard acquisition techniques. 76 91.1
105.1 132.1
171.1
However, tMRM acquisition gave valuable qualitative data that could be used
in library matching for definitive confirmation. -1
117
145
9.663 x103 117

9.618 tMRM Library Spectrum
x104 QC 50 ppb 41289 x104 150839 Blank Ginger Extract 1
RT 9.663 min
145 Tebufenpyrad
3
RT 9.618 min (- 0.47 %)
1
Qual/Quant ratio 89.8 % Calc. Conc. 185 µg/kg
H3C
Qual/Quant ratio CH3
2 H3C
110.6 % (123.1 %) Cl
0.5 0.5
H3C N
1 NH
76 91.1 N
105.1 132.1
0 0 171.1 O CH3
x104 9.663 334.2
37093 x104 9.619
4 166829 0
80 100 120 140 160 180 200 220 240 260 280 300 320 340
1
3
0.5
2 Figure 5. Library match result for the native ginger compound searched against
1 the tMRM library spectrum for tebufenpyrad yielded a library match score
of 70.34, allowing rejection of the native compound as tebufenpyrad and
0 0
9.45 9.5 9.55 9.6 9.65 9.7 9.75 9.8 9.45 9.5 9.55 9.6 9.65 9.7 9.75 9.8 avoiding a positive result.
Counts vs. Acquisition Time (min) Counts vs. Acquisition Time (min)
Figure 4. Primary MRM traces for tebufenpyrad in 50 ppb quality control standard CONCLUSIONS
(left) and in a ginger extract (right). The top chromatograms represent The analyses of pesticides in chamomile and ginger extracts with tMRM
the quantifier traces for tebufenpyrad (m/z 334.1 > 117.1) and the bottom acquisition achieved accurate quantitative analysis with the confidence of
chromatograms represent the first qualifier traces (m/z 334.1 > 145.1) library matching in a single analytical run. Tebuthiuron and tebufenpyrad were
successfully distinguished from nearby or co-eluting endogenous compounds,
and false positives were successfully averted with the inclusion of qualitative
Figure 5 shows the library search results for the native ginger compound
analysis with library matching. tMRM acquisition is a data-dependent scan
with similar retention time, quantifier, and qualifier ions to tebufenpyrad. The
mode capable of providing quantitative and qualitative data on a single
bottom window shows the stored library spectrum and the upper window
instrument, in a single injection.
shows the spectrum that has been acquired for the native ginger compound.
The mirrored spectra in the central window allowed for a simple comparison of REFERENCES
the acquired versus the library spectrum. Although this co-eluting compound (1) Regulation (EC) No. 396/2005 of the European Parliament and of the Council
would commonly give a false positive result in typical quantitative MRM of 23 February 2005 on maximum residue levels of pesticides in or on food
analyses, we see here that there are many peaks present in the tebufenpyrad and feed of plant and animal origin and amending Council Directive 91/414/
tMRM library spectrum that were missing from the native ginger compound
EEC (including amendments as of 18 March 2008).
spectrum. As a result, the library match score was only 70.34 out of 100, and
(2) European Guideline SANCO/10684/2009: Method validation and quality
we were able to confidently reject the native compound as tebufenpyrad.
control procedures for pesticide residues analysis in food and feed.
(3) Official collection of test procedures according to §64 law on food and animal
feed (LFGB), Beuth-Verlag.

Published in USA
30 Fatty Acids AGILENT TECHNOLOGIES APPLICATION NOTEBOOK
Analysis of Plant Stanyl Fatty Acid Esters in Enriched Margarine

Using an Online Coupled Agilent 1220 Infinity LC-7890 GC System
Andreas Barnsteiner, Rebecca Esche, Karl-Heinz Engel, Munich Technical University, Freising, Germany
Walter Kohlert, Stefan Fenzel, Agilent Technologies, Inc., Waldbronn, Germany
ABSTRACT EXPERIMENTAL
The work described here involved the investigation of intact plant stanyl fatty acid Chemicals and materials
esters in an enriched commercial margarine using an online coupled Agilent 1220 The plant stanyl ester mixture “plant stanol ester, STAEST-115” was provided
Infinity LC-7890A GC system. The lipid extract was directly analyzed without prior by Raisio Group (Raisio, Finland). The internal standard cholesteryl palmitate
purification steps. The LC fraction of plant stanyl esters was transferred online (≥ 98%) was obtained from Sigma Aldrich (Taufkirchen, Germany).
into the GC system using the solvent vent mode of the multimode inlet for solvent
Benecol (taste-type Kevyt kasvirasvalevite 32%, with added plant stanyl
evaporation. The online LC-GC combination showed very good linearity and
esters) margarine was purchased in a supermarket in Finland. The plant
repeatability.
stanol content was labeled as 8 wt-%, total lipids as 32 wt-%.
INTRODUCTION
Plant steryl and stanyl esters (Figure 1) are added to food products like
skimmed milk-drinking yogurts or margarines because of their cholesterol-
lowering properties. The capillary gas chromatographic investigation of plant
stanyl fatty acid esters from skimmed milk products can be performed directly
after the lipid extraction1. However, the presence of di- and triglycerides may RO RO
hamper the direct GC quantification. Therefore, the analysis in lipid extracts
from foods with high fat contents like margarine requires a fractionation Campestanyl- Sitostanyl-
prior to the GC separation by laborious offline techniques, such as Thin Layer
O
Chromatography (TLC) or Solid Phase Extraction (SPE). The online coupling of
R= 16:0
LC and GC offers an efficient and elegant alternative. The plant stanyl esters
can be fractionated by liquid chromatography and transferred online into O
the GC system. In this way, the pre-fractionation step and the capillary gas 18:0
chromatographic analysis of the transferred LC fraction are performed in a O
closed system in one run. Hence, the risk of sample loss and contamination is 18:1
reduced and the approach results in better repeatability2, 3.
O
In a recently published paper1, the analysis of plant stanyl esters in enriched 18:2
margarines using an online LC-GC system equipped with a loop-type interface O
was reported. Using the loop-type interface, the solvent evaporation was 18:3
performed in the GC capillary columns by means of a pre-column system in
O
combination with an early solvent vapor exit. Due to the high solvent amounts
20:0
which were loaded on the pre-column system with each transfer, a loss of
resolution was observed after a few runs.
Figure 1. Structures of plant stanyl fatty acid esters
The online coupling of an Agilent 1220 Infinity LC system and an Agilent
7890A GC system, with a 2-position/6-port switching valve using the solvent SAMPLE PREPARATION OF MARGARINE1
vent mode of the multimode inlet of the GC, allowed for the evaporation The margarine sample (20–40 mg, accuracy of ± 0.1 mg) was weighed
of the solvent prior to the capillary column4. A pre-column system and/or a into a vessel; internal standard (cholesteryl palmitate, 750 µg), 5 mL
solvent vapor exit were not necessary. This combination was already suitable of n-hexane/MTBE (3:2) and sodium sulfate (anhydrous) were added
for the analysis of cholesteryl esters4. and sonicated for 1 minute. The solution was filtered through a 0.45
The use of an Agilent online coupled LC-GC combination for the quantification μm membrane filter assembled with a 5 mL syringe. The vessel and
of plant stanyl esters in enriched margarine is presented here. the filter were washed twice with 5 mL n-hexane/MTBE (3:2). After
dilution (1:5) of the combined extracts, the solution was used for
online LC-GC analysis.
AGILENT TECHNOLOGIES APPLICATION NOTEBOOK Fatty Acids 31
QUANTIFICATION
The five-point calibration functions of nine individual stanyl esters were
generated in a range of 0.2 – 1.0 μg of total stanyl ester (“plant stanol ester,
STAEST-115”) per 2 μL i.v. Each calibration point was done in triplicate. Linear
regression analysis was performed in coordinate ratios of areas (individual
stanyl ester/IS) and amounts (individual stanyl ester/IS).
EQUIPMENT
The coupling of the Agilent 1220 Infinity LC system to the Agilent 7890A GC
system was accomplished using an Agilent 2-position/6-port switching valve
equipped with a 200 µL sample loop (Table 1). The evaporation of the eluent
was performed using the temperature programmable MultiMode (MM) Inlet
in the Programmable-Temprature Vaporizing (PTV) solvent vent mode4.
Table 1. Liquid and gas chromatographic conditions

CHROMATOGRAPHIC CONDITIONS
LC conditions
Injection 2 µL
volume:
Eluent: n-hexane/tert-butylmethyl ether (96:4, v/v)
Column 27 °C
temperature:
Column flow: 0.200 mL/min
Column type: Eurospher-100Si (250 x 2 mm id, 5 µm)
Wavelength: 205 nm
LC controlled interface
Transfer valve: 4.25 min: Position 1 & 2
7.50 min: Position 2 & 1
GC start: 4.20 min: Change contacts switch contact A to closed
4.25 min: Change contacts switch contact A to open
GC conditions
Front MM inlet: Mode: Solvent vent
Carrier: H2
Pressure: 7.8 psi
Septum purge flow: 3 mL/min
Vent pressure: 4 psi until 0.5 min
Vent flow: 1000 mL/min
Temperature program: Initial: 50 °C for 0.5 min
Rate 1: 900 °C/min to 350 °C for 2 min
Purge flow to split vent: 2.5 mL/min at 0.5 min
Gas saver: 20 mL/min after 5 min
Column 1: Column type: Restek Rtx-200MS: 30 m × 250 µm; 0.1 µm df;
Constant flow: 1.5 mL/min
Column 2: Transfer line, controlled by PCM C-1

Pressure program: Initial: 5 psi for 0.3 min
Rate 1: 10 psi/min to 20 psi
Oven: Temperature program: Initial: 40 °C for 2 min
Rate 3: 1.5 °C/min to 340 °C for 3 min
Detector: FID: 360 °C
(H2: 30 mL/min, Air: 400 mL/min; Makeup: 25 mL/min)
32 Fatty Acids AGILENT TECHNOLOGIES APPLICATION NOTEBOOK
RESULTS AND DISCUSSION

The chromatograms obtained by online LC-GC analysis of a margarine enriched (a) mAU
14
with plant stanyl esters are presented in Figure 2. The LC-fractionation (Figure 12
2a) was performed isocratically on a silica gel column with n-hexane/MTBE 10
(96+4; v+v) as mobile phase. The plant stanyl esters eluted after approximately 8
6
Transfer window
4 minutes. The transfer was performed 4.25 minutes after injection. The 4
transfer conditions for the analysis of cholesteryl esters4 were also suitable for 2
plant stanyl esters. The GC separation of the transferred fraction was similar
0
0 5 10 15 20 25 30 min
to that reported for the online LC-GC analysis via a loop-type interface1. The (b)
pA
pA
(b)
intact plant stanyl fatty acid esters were distinguishable according to their 12
12 6
6
carbon number and, in the case of unsaturated fatty acid moieties, to the 10
10
IS
number of double bonds; only the esters of saturated and monounsaturated 8
8 IS
3 7
fatty acids of the same chain length eluted at the same time. 6
6 3 7
4
44 22 4 8
11 5 58 9 9
Under the employed online LC-GC conditions, using the Agilent Multimode 22
Inlet for the solvent evaporation4, the solvent load on the GC capillaries was 00
00 55 10
10 15
15 20
20 2525 3030 min
min
low in comparison to the loop-type coupled system. Even after 600 transfers,
no loss of resolution was observed using the online LC-GC combination. Figure 2. Analysis of plant stanyl esters in enriched margarine by online LC-GC/
FID; (a) LC-chromatogram and (b) GC-chromatogram of the transferred
For the calibration, linear regression analysis was performed in the coordinate LC-fraction; peak numbering according to Table 2; (IS) internal standard
ratios of areas (individual stanyl ester/IS) and amounts (individual stanyl cholesteryl palmitate
ester/IS). The correlation coefficients of the calculated calibration functions
(R²) were in the range of 0.995 – 0.999, showing very good linearity of the
online LC-GC/FID detector response.
The repeatability was determined by 10-fold injections of the same sample
solution. The coefficients of variation were low (< 9%) for all plant stanyl
esters (Table 2). The quantitative results were comparable to those obtained
by means of the loop-type interface coupled online LC-GC1.
Table 2 Coefficients of variation of plant stanyl esters

CV [%]b
No. a
Stanyl ester Extract 1 Extract 2 Extract 3 Amount [g/100 g]c
1 Campestanyl-16:0/16:1 7.7 2.0 5.1 0.18 ± 0.01 (8.1)
2 Sitostanyl-16:0/16:1 5.7 0.7 2.6 0.47 ± 0.02 (5.3)
3 Campestanyl-18:0/18:1 1.1 0.8 0.6 2.10 ± 0.06 (2.8)
4 Campestanyl-18:2 3.7 1.6 3.2 0.73 ± 0.04 (5.2)
5 Campestanyl-18:3 8.8 2.8 6.9 0.30 ± 0.02 (7.6)
6 Sitostanyl-18:0/18:1 1.1 0.9 1.5 6.36 ± 0.22 (3.5)
7 Sitostanyl-18:2 1.9 1.5 2.0 2.17 ± 0.11 (5.1)
8 Sitostanyl-18:3 6.5 2.2 7.2 0.81 ± 0.06 (8.0)
9 Sitostanyl-20:0/20:1 4.8 2.5 5.5 0.19 ± 0.01 (7.0)
Total stanyl esters 1.6 0.7 1.6 13.3 ± 0.5 (3.7)
Esterified sterols 1.6 0.7 1.6 8.1 ± 0.3 (3.7)
a
Peak number correspond to Figure 2b
b
Coefficient of variation [CV] determined by 10-fold injections of the same sample solution
c
Values represent average ± standard deviations of 30 analyses (coefficient of variation [%])
AGILENT TECHNOLOGIES APPLICATION NOTEBOOK Fatty Acids 33
CONCLUSION
Online coupling of an Agilent 1220 Infinity LC system and an Agilent 7890A
GC system was shown to be suitable for the quantitative analysis of plant
stanyl fatty acid esters in enriched margarine. The online LC-GC system was
characterized by easy handling and a very robust separation performance
for both dimensions. Therefore, the Agilent online LC-GC combination can
be a valuable tool for the routine analysis of plant steryl and stanyl esters in
functional foods.
REFERENCES
(1) A. Barnsteiner, T. Lubinus, A. di Gianvito, W. Schmid, K.-H. Engel, GC-Based
Analysis of Plant Stanyl Fatty Acid Esters in Enriched Foods. Journal of
Agricultural and Food Chemistry, 2011, 59, (10), 5204-5214.
(2) P. Dugo, G. Dugo, L. Mondello, On-line coupled LC-GC: theory and applications.
LC-GC Eur. 2003, 16, (12a), 35-43.
(3) T. Hyoetylaeinen, M.-L. Riekkola, On-line coupled liquid chromatography-gas
chromatography. J Chromatogr A 2003, 1000, (1-2), 357-84.
(4) R. Esche, A. Barnsteiner, K.-H. Engel, W. Kohlert, S. Fenzel, Two-dimensional
chromatography: LC-GC online coupling of on Agilent 1260 Infinity LC and an
Agilent 7890A GC, Agilent Technical Overview, publication number 5990-
8025EN; 2011

Published in USA
READY TO GO FOR PESTICIDES AND
ENVIRONMENTAL POLLUTANTS
Triple Quadrupole GC/MS Multiresidue Analyzer
Agilent Analyzers and Applications Kits
Fully configured and factory chemically-

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• Retention Time Locked HP-5MS Ultra Inert column for reliable
peak identification and quantitation
• Checkout samples of 17 representative analytes
• Capillary Flow Technology and backflush for reduced maintenance
• Quick-start guide that allows you to quickly utilize Agilent
advanced technologies and get high performance analytical
results on day one
• CD-ROM with system-specific checkout data files and reports
Boost your multiresidue screening productivity
Perform highly sensitive, multiresidue target
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Flexible, comprehensive MRM Database Top two transitions
Orange
Orange Pear
Pear
contains over 1000 pesticides and pollutants, and is of Methamidophos
optimized with an average of 8 MRM transitions to
minimize matrix interference. It also includes a tool that 141.0
141.0 95.0
95.0
makes it easy to build methods based on your own list.
95.0
95.0 79.0
79.0
Integrated Capillary Flow Technology (CFT) medium matrix interference strong matrix interference
(overlapping peak gives incorrect (overlapping peak gives
backflush promotes shorter analysis times, lower ion ratio) inaccurate quantitation result)
chemical background, longer column life, and less
frequent ion source cleaning to improve uptime. Orange
Orange Pear
Pear
Two alternative transitions
of Methamidophos
95.0
95.0 64.0
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Multimode inlet (MMI) with large-volume
injection enhances trace-level detection and
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adds flexibility by including hot or cold
split/splitless capabilities. minimum matrix interference minimum matrix interference
The G9250AA database has on average 8 transitions for each compound.

This allows the user to choose alternative transitions to minimize matrix interferences
x104
0.9
Ratio=23.3 Superior GC/MS/MS selectivity and and improve quantitation results.
sensitivity eliminates false results, and simplifies
0.8
0.7
0.6
Counts
0.5
data review for improved productivity.

0.4
0.3
0.2
0.1
0
Ordering information:
12.20 12.30 12.40 12.50 12.60 12.70 12.80 11.8 11.9 12 12.1 12.2 12.3
me Aquisition Time (min)
x103
Ratio=23.6
8
7
6
5
Counts
Choose one of the following options when you order an

4
3
2
1
Agilent 7000 Series Triple Quadrupole GC/MS with an

0
0 12.20 12.30 12.40 12.50 12.60 12.70

me
11.8 11.9 12 12.1
Aquisition Time (min)
12.2 12.3
Productivity tools to help you make the most

out of every analysis: Agilent autotune, batch-at- Agilent 7890A GC analyzer system:
x104 Ratio=24.0
1.2
1.1
1
0.9
a-glance data review, and parameter-less integrator

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Counts
• The flexibility-driven setup. G3445A Option 411:

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streamline your data review and processing.

0.3
0.2
0.1
GC/MS/MS Pesticide and Environmental Pollutant Analyzer with

0
-0.1
12.20 12.30 12.40 12.50 12.60 12.70 12.80 11.8 11.9 12 12.1 12.2 12.3
me Aquisition Time (min)
constant pressure, post-column backflush method

• The performance-driven setup. G3445A Option 412:
GC/MS/MS Pesticide and Environmental Pollutant Analyzer with
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For customers who already own an Agilent GC/QQQ system:
• G9250AA: Pesticides and Environmental Pollutants MRM database
Agilent also offers Single Quadrupole GC/MSD pesticide analyzers for broad screening at
5 to 100 ppb. Each is equipped with CFT Backflush, Deconvolution Reporting Software,
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brochure 5990-5310EN, for details.

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Information, descriptions and specifications

in this publication are subject to change
without notice.
© Agilent Technologies Inc. 2012

Published April 16, 2012
5991-0348EN

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Application Notebook

AGILENT FOOD TESTING SOLUTIONS

Food Safety Summit:

© Agilent Technologies, Inc. 2012

Cost-effective Analysis of Major, Minor and Trace Elements

Determination of Fatty Acid Methyl Esters (FAMEs) in

Method for the Determination of Chemical Contaminants

Analysis of Medium Volatility Sulfur Compounds in Coffee

Simple, Rapid Analysis of Trace Metals in Foods Using the

A Reliable and Routine GC/MS/MS Method for the Determination

A Prediction Model for Determining Wine Variety using the

Triple Quadrupole LC/MS Analysis of Aflatoxins in Various Food Samples. . . . . . . 25

Identification and Quantitation of Pesticides in Chamomile and

Analysis of Plant Stanyl Fatty Acid Esters in Enriched Margarine

© Agilent Technologies, Inc. 2012

Gas Chromatography with Capillary Flow Technology

SOLUTIONS AND STANDARDS SAMPLE PREPARATION

of ACN to yield a 50 mg/mL concentration. The appropriate amount of

gulonolactone solution was added to the calibration standards to yield a 0.5

QuEChERS Sample Preparation Workflow 1400000

Weigh 3 g sample (± 0.05 g) 50 mL centrifuge tube 1000000

© Agilent Technologies, Inc. 2012

Cost-Effective Analysis of Major, Minor, and Trace Elements

Table 3. Results of NIES No.7 Tea Leaves

Table 4. Results of NIES No.10c Rice Flour

Table 5. Results of NIST 1577 Bovine Liver

Table 6. Results of CRM-Wheat Flour

Table 7. Results of CRM-Milk Powder Table 8. Results of CRM-Oyster Tissue

© Agilent Technologies, Inc. 2012

Determination of Fatty Acid Methyl Esters (FAMEs) in Salmon Oil

MATERIALS AND METHODS

Table 1. GC/FID Conditions Flag empty vial as Result

RESULTS AND DISCUSSION

Table 2. Percent distribution of fatty acids in salmon oil sample

© Agilent Technologies, Inc. 2012

Method for the Determination of Chemical Contaminants

INTRODUCTION KEY BENEFITS

© Agilent Technologies, Inc. 2012

Analysis of Medium Volatility Sulfur Compounds

concentrations at ng/mL levels naturally occurring in coffee extract. 1

In summary, an Agilent 7200 GC/Q-TOF system is able to provide trace-level

© Agilent Technologies, Inc. 2012

Simple, Rapid Analysis of Trace Metals in Foods

Set by Autotune CeO+/Ce+ (%) 1.114

Traditionally, covering this range of concentrations for these elements would

Scan the QR code for more information

© Agilent Technologies, Inc. 2012

NRC-CNRC DORM3 NIST SRM 2976 NIST RM 8415

Certified value Measured Certified value Measured Certified value Measured

23 Na – – – – 3770 ± 340 3807

© Agilent Technologies, Inc. 2012

A Reliable and Routine GC/MS/MS

ASSURE Agilent Technologies, Inc.

To learn more about Agilent sample

© Agilent Technologies, Inc. 2012

To learn more about LC/MS and

A Prediction Model for Determining Wine

To learn about OpenLAB Informatics

© Agilent Technologies, Inc. 2012

• The flexibility-driven setup. G3445A Option 411: