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Accurate, stable and fast analysis of toxic inorganic arsenic (iAs) in complicated and arsenosugar-rich algae matrix is always a challenge. Herein, a novel analytical method for iAs in algae was reported, using bromine halogenation and... more
Accurate, stable and fast analysis of toxic inorganic arsenic (iAs) in complicated and arsenosugar-rich algae matrix is always a challenge. Herein, a novel analytical method for iAs in algae was reported, using bromine halogenation and on-line nonpolar solid phase extraction (SPE) followed by hydride generation atomic fluorescence spectrometry (HG-AFS). The separation of iAs from algae was first performed by nonpolar SPE sorbent using Br(-) for arsenic halogenation. Algae samples were extracted with 1% perchloric acid. Then, 1.5mL extract was reduced by 1% thiourea, and simultaneously reacted (for 30min) with 50μL of 10% KBr for converting iAs to AsBr3 after adding 3.5mL of 70% HCl to 5mL. A polystyrene (PS) resin cartridge was employed to retain arsenicals, which were hydrolyzed, eluted from the PS resin with H2O, and categorized as iAs. The total iAs was quantified by HG-AFS. Under optimum conditions, the spiked recoveries of iAs in real algae samples were in the 82-96% range, and...
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A rugged, filter-based fluorometer capable of time-resolved luminescence (TRL) measurements was designed, prototyped and tested for field applications. The instrument operation and data processing were controlled by a laptop computer... more
A rugged, filter-based fluorometer capable of time-resolved luminescence (TRL) measurements was designed, prototyped and tested for field applications. The instrument operation and data processing were controlled by a laptop computer running a custom LabVIEW program. A xenon flashlamp was used as the light source and a photomultiplier tube (PMT) as the photodetector. A gating technique was implemented to effectively overcome PMT saturation by intense xenon lamp flash so signal integrity was maintained even at very high gains, leading to improved sensitivity and reproducibility. The instrument was tested by TRL using tetracycline as a model analyte; and the signal was digitized at a 2-mus time resolution and a 12-bit amplitude resolution. Its performance was similar to or slightly better than that of a commercial fluorescence spectrophotometer. A 0-300 ppb linear dynamic range (r2 = 0.9996) and a 0.025-ppb limit of detection (LOD) were achieved with a <=5% relative standard deviation.
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A novel dielectric barrier discharge reactor (DBDR) was utilized to trap/release arsenic coupled to hydride generation atomic fluorescence spectrometry (HG-AFS). On the DBD principle, the precise and accurate control of trap/release... more
A novel dielectric barrier discharge reactor (DBDR) was utilized to trap/release arsenic coupled to hydride generation atomic fluorescence spectrometry (HG-AFS). On the DBD principle, the precise and accurate control of trap/release procedures was fulfilled at ambient temperature, and an analytical method was established for ultratrace arsenic in real samples. Moreover, the effects of voltage, oxygen, hydrogen and water vapor on trapping and releasing arsenic by DBDR were investigated. For trapping, arsenic could be completely trapped in DBDR at 40 mL/min of O2 input mixed with 600 mL/min Ar carrier gas and 9.2 kV discharge potential; prior to release, the Ar carrier gas input should be changed from the upstream gas liquid separator (GLS) to the downstream GLS and kept for 180 s to eliminate possible water vapor interferences; for arsenic release, O2 was replaced by 200 mL/min H2 and discharge potential was adjusted to 9.5 kV. Under optimized conditions, arsenic could be detected as...
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Residues of malachite green (MG), gentian violet (GV), and their leuco metabolites in channel catfish muscle were individually determined by HPLC using diode array and fluorescence detectors and confirmed by tandem mass spectrometry. This... more
Residues of malachite green (MG), gentian violet (GV), and their leuco metabolites in channel catfish muscle were individually determined by HPLC using diode array and fluorescence detectors and confirmed by tandem mass spectrometry. This detection scheme obviates a PbO(2) reactor that converts leuco forms to chromatic forms for absorbance detection, therefore eliminating uncertainties in oxidant depletion and data integrity. Extraction was performed once in pH 3 McIlvaine buffer and acetonitrile, followed by cleanup using a polymeric strong cation-exchange column. Liquid-liquid extraction was excluded to provide an environmentally responsible and relatively rapid protocol. Spectrometric limits of detection (LOD; S/N = 3) for MG (lambda = 620 nm) and GV (lambda = 588 nm) were 0.38 and 0.26 ng/g with 44.5-49.2% and 92.2-101.4% recoveries (1-10 ng/g, n = 6), respectively. Fluorometric LOD (S/N = 3) for LMG and LGV (lambda(ex) = 266 nm, lambda(em) = 360 nm) were 0.10 and 0.09 ng/g with 74.3-84.5% and 80.6-86.5% recoveries (1-10 ng/g, n = 6), respectively. This simplified protocol saves costs and meets the sensitivity requirements set by the Food and Drug Administration and the European Union.
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Three neutral cyclophanes were synthesized, and their association with indole, an aromatic pi-donor, was studied. The cyclophanes were designed to contain a rigid, hydrophobic binding cavity with 1,4,5,8-naphthalenetetracarboxylic diimide... more
Three neutral cyclophanes were synthesized, and their association with indole, an aromatic pi-donor, was studied. The cyclophanes were designed to contain a rigid, hydrophobic binding cavity with 1,4,5,8-naphthalenetetracarboxylic diimide or 1,5-dinitronaphthalene as the pi-acceptor. Two of the cyclophanes also contain a (S)-(valine-leucine-alanine) tripeptide unit to provide chiral hydrogen bonding interactions with guest molecules. Despite the fact that these cyclophanes contain a hydrophobic binding cavity of appropriate dimensions, their association with indole is very weak. In the case of cyclophanes derived from 1,5-dinitronaphthalene, steric interactions force the nitro groups out of the plane of the naphthalene ring, diminishing their effectiveness as pi-acceptors. A simple UV--visible titrimetric method, using N,N,N&#39;,N&#39;-tetramethyl-1,4-phenylenediamine (TMPD) as a pi-donor, was used to rank the pi-acceptor strength of these and other aromatic units. These titrations show that 1,4,5,8-naphthalenetetracarboxylic diimide and 1,5-dinitronaphthalene derivatives are weaker pi-acceptors than viologens, which make good pi-acceptor cyclophanes. Methyl viologen is in turn a weaker pi-acceptor than anthaquinone disulfonate, suggesting that the latter may serve as a useful building block for pi-accepting cyclophane hosts.
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Oxytetracycline (OTC) is extensively used in aquaculture worldwide for preventive and therapeutic purposes. Most of the drug, however, is discharged into the marine environment due to leaching from medicated feed and poor gastrointestinal... more
Oxytetracycline (OTC) is extensively used in aquaculture worldwide for preventive and therapeutic purposes. Most of the drug, however, is discharged into the marine environment due to leaching from medicated feed and poor gastrointestinal (GI) absorption. Without exposure to sun light OTC has a long lifetime in the marine environment, therefore it is important to monitor and study its occurrence, distribution,
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... 1 Botany Department, PO Box 3165, Chemistry Department, University of Wyoming, Laramie, WY 82071, USA. a University of Wyoming, Laramie, WY 82071, USA. Available online 11 April 2008. Excerpt. Note: This is a one-page preview only.... more
... 1 Botany Department, PO Box 3165, Chemistry Department, University of Wyoming, Laramie, WY 82071, USA. a University of Wyoming, Laramie, WY 82071, USA. Available online 11 April 2008. Excerpt. Note: This is a one-page preview only. Click here to download preview. ...
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A sensitive method was developed to speciate and quantify As(III) and As(V) in fruit juices. At pH 3.0, As(III) and ammonium pyrrolidine dithiocarbamate (APDC) formed a complex, which was extracted into CCl4 by dispersive liquid-liquid... more
A sensitive method was developed to speciate and quantify As(III) and As(V) in fruit juices. At pH 3.0, As(III) and ammonium pyrrolidine dithiocarbamate (APDC) formed a complex, which was extracted into CCl4 by dispersive liquid-liquid microextraction (DLLME) and subsequently quantified by hydride generation-atomic fluorescence spectrometry (HG-AFS). After As(V) was reduced by thiosulphate at pH 1.7-1.8, total inorganic arsenic (iAs) was determined following the same protocol and As(V) was calculated from the difference. Interference from methylarsonic acid (MMA) was managed at &amp;amp;amp;amp;amp;amp;amp;amp;amp;amp;lt;10% by controlling the pH of the reduction reaction. This procedure achieved 1.2μgL(-1) limit of detection (3σ) and 92-102% recovery at 10μgL(-1), and is applicable to most fruit juices except certain pear juice that may contain considerable MMA.
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A rugged, filter-based fluorometer capable of time-resolved luminescence (TRL) measurements was designed, prototyped and tested for field applications. The instrument operation and data processing were controlled by a laptop computer... more
A rugged, filter-based fluorometer capable of time-resolved luminescence (TRL) measurements was designed, prototyped and tested for field applications. The instrument operation and data processing were controlled by a laptop computer running a custom LabVIEW program. A xenon flashlamp was used as the light source and a photomultiplier tube (PMT) as the photodetector. A gating technique was implemented to effectively overcome PMT saturation by intense xenon lamp flash so signal integrity was maintained even at very high gains, leading to improved sensitivity and reproducibility. The instrument was tested by TRL using tetracycline as a model analyte; and the signal was digitized at a 2-mus time resolution and a 12-bit amplitude resolution. Its performance was similar to or slightly better than that of a commercial fluorescence spectrophotometer. A 0-300 ppb linear dynamic range (r2 = 0.9996) and a 0.025-ppb limit of detection (LOD) were achieved with a <=5% relative standard deviation.
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Oxytetracycline (OTC) residue in honey is detected using a portable analyzer designed to specifically target tetracycline (TC) drugs based on europium-sensitized luminescence (ESL). A 385 nm light emitting diode (LED) is used as the... more
Oxytetracycline (OTC) residue in honey is detected using a portable analyzer designed to specifically target tetracycline (TC) drugs based on europium-sensitized luminescence (ESL). A 385 nm light emitting diode (LED) is used as the excitation source and a photomultiplier tube as the light detector. OTC is extracted from honey and cleaned up by solid phase extraction (SPE) using Strata X-WC
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In this study, the slurry sampling hydride generation (SLS-HG) system was first coupled with in situ dielectric barrier discharge atomic fluorescence spectrometry (DBD-AFS) for arsenic analysis in biological samples based on the gas phase... more
In this study, the slurry sampling hydride generation (SLS-HG) system was first coupled with in situ dielectric barrier discharge atomic fluorescence spectrometry (DBD-AFS) for arsenic analysis in biological samples based on the gas phase enrichment (GPE) principle.
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Hyphenation of sorbent extraction and solid-matrix time-resolved luminescence (TRL) was demonstrated using tetracycline (TC) in milk as a model analyte. The performance of a C18-impregnated silica layer was evaluated as both an extraction... more
Hyphenation of sorbent extraction and solid-matrix time-resolved luminescence (TRL) was demonstrated using tetracycline (TC) in milk as a model analyte. The performance of a C18-impregnated silica layer was evaluated as both an extraction sorbent and a TRL substrate. To extract TC, a 10 x 6 mm glass-backed C18 layer was dipped into a 10 mL milk sample for 10 min followed by a 3-min water immersion for cleanup. The sorbent was then spotted with a TRL reagent solution at pH 9 that contained 5 mM europium nitrate and 5 mM EDTA. After a brief desiccation period, TRL was measured directly on the sorbent surface with a commercial fluorescence spectrophotometer. By eliminating the need to elute the analyte from the sorbent, organic solvent was not needed and sample preparation was greatly simplified. The integrated signal showed a linear dependence (R(2) = 0.9938) on TC concentration in the 0-3000 microg/L range. The same protocol was applicable to screening TC in fat-free, 2% low-fat, and whole milk at 300 microg/L, the US. regulatory tolerance level set by the Food and Drug Administration (FDA). This easy, fast, and low-cost screening method is friendly to the environment and particularly suitable for liquid samples.
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A luminescence method was developed to screen residues of enrofloxacin (ENRO) and its metabolite, ciprofloxacin (CIPRO), in swine liver. Target analytes were extracted in acetonitrile/1.5% trifluoroacetic acid/NaCl, cleaned up by... more
A luminescence method was developed to screen residues of enrofloxacin (ENRO) and its metabolite, ciprofloxacin (CIPRO), in swine liver. Target analytes were extracted in acetonitrile/1.5% trifluoroacetic acid/NaCl, cleaned up by dispersive liquid-liquid microextraction (DLLME), and finally detected by terbium-sensitized luminescence (TSL) using a time-resolved luminescence photometer. CIPRO yielded slightly lower TSL response than ENRO, so a common threshold was derived from CIPRO and applied to both fluoroquinolones. Among 37 samples randomly spiked with CIPRO or ENRO up to 1 μg/g, all 19 samples spiked above the 500 ng/g tolerance were correctly screened as positive with no false negatives, but 3 of 18 samples spiked below 500 ng/g were classified as positive. This method minimized the use of chlorinated solvents and significantly improved sample throughput.
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Analyses of chemical residues in animal tissue matrices require multistep sample preparation. To simplify this process, a methodology was developed that combines sorbent extraction and solid-matrix time-resolved luminescence (TRL); it was... more
Analyses of chemical residues in animal tissue matrices require multistep sample preparation. To simplify this process, a methodology was developed that combines sorbent extraction and solid-matrix time-resolved luminescence (TRL); it was applied to tetracycline screening in milk. Reported here is an effort to extend its application to tissue matrices, illustrated by oxytetracycline (OTC) screening in catfish muscle. Extraction and enrichment are accomplished by immersing small C18 sorbent strips into tissue homogenates for 20 min, followed by a 3 min rinse in water and a 2 min dip in a reagent solution. After desiccation, TRL is measured directly on the sorbent surface. Tissue particulates no longer interfere via attenuation or scattering, rendering centrifugation and filtration unnecessary. The integrated TRL intensity shows a linear dependence on OTC concentration in the 0-8 microg/g range (R2 = 0.9992) with a 0.026 microg/g limit of detection. To screen OTC at 2 microg/g, the U.S. regulatory tolerance level, a threshold is established at x2-3sigma2, where x2 and sigma2 are the mean and standard deviation, respectively, of the TRL signals from 15 samples fortified at 2 microg/g. Among 45 blind samples randomly fortified at 0-4 microg/g, 41 were screened correctly and 4 negative samples were presumed positive. This method has the potential to improve throughput and save assay costs by eliminating acids, organic solvents, centrifugation, and filtration.
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Research Interests: Perfume, Pharmaceutical Technology, Drug delivery, Adsorption, Controlled release, and 11 moreDiffusion, Viscosity, Esterification, Gels, Pharmaceutical Formulation Technology, Pectins, Monoterpenes, Delayed-Action Preparations, Volatilization, Aldehydes, and Pharmacology and pharmaceutical sciences
A luminescence photometer was developed based on lanthanide-sensitized luminescence to detect environmental pollutants and residues in foods including, in particular, two classes of antibiotics: tetracyclines and fluoroquinolones.... more
A luminescence photometer was developed based on lanthanide-sensitized luminescence to detect environmental pollutants and residues in foods including, in particular, two classes of antibiotics: tetracyclines and fluoroquinolones. Multiple excitation sources, a xenon flashlamp and ultraviolet light-emitting diodes (UV LEDs), were used to their advantages. A photomultiplier tube module, gated to reject time-domain interferences, was used as a photodetector. Using danofloxacin as a model analyte, luminescence signal was linear in more than three decades (0.5–2000 ng/mL) with R 2 > 0.998 in each decade. This photometer achieved a limit of detection of 2.0 ng/mL with 1.3% average relative standard deviation. It is field deployable at 4.6 kg and 15 W power consumption.
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... Methods have been developed for analysis of the tetracyclines in poultry, however, these methods may be lengthy and/or require expensive instrumentation.22. Capolongo, F., Santi, A., Tomasi, L., Anfossi, P., Missagia, M. and... more
... Methods have been developed for analysis of the tetracyclines in poultry, however, these methods may be lengthy and/or require expensive instrumentation.22. Capolongo, F., Santi, A., Tomasi, L., Anfossi, P., Missagia, M. and Montesissa, C ... Schneider, MJ and Lehotay, SJ 2004 ...
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Residues of malachite green (MG), gentian violet (GV), and their leuco metabolites in channel catfish muscle were individually determined by HPLC using diode array and fluorescence detectors and confirmed by tandem mass spectrometry. This... more
Residues of malachite green (MG), gentian violet (GV), and their leuco metabolites in channel catfish muscle were individually determined by HPLC using diode array and fluorescence detectors and confirmed by tandem mass spectrometry. This detection scheme obviates a PbO(2) reactor that converts leuco forms to chromatic forms for absorbance detection, therefore eliminating uncertainties in oxidant depletion and data integrity. Extraction was performed once in pH 3 McIlvaine buffer and acetonitrile, followed by cleanup using a polymeric strong cation-exchange column. Liquid-liquid extraction was excluded to provide an environmentally responsible and relatively rapid protocol. Spectrometric limits of detection (LOD; S/N = 3) for MG (lambda = 620 nm) and GV (lambda = 588 nm) were 0.38 and 0.26 ng/g with 44.5-49.2% and 92.2-101.4% recoveries (1-10 ng/g, n = 6), respectively. Fluorometric LOD (S/N = 3) for LMG and LGV (lambda(ex) = 266 nm, lambda(em) = 360 nm) were 0.10 and 0.09 ng/g with 74.3-84.5% and 80.6-86.5% recoveries (1-10 ng/g, n = 6), respectively. This simplified protocol saves costs and meets the sensitivity requirements set by the Food and Drug Administration and the European Union.