Int. J. Pharm. Sci. Rev. Res., 59(1), November - December 2019; Article No.

04, Pages: 17-21 ISSN 0976 – 044X

Research Article

Determination of Methyl Paraben from Cosmetics by UV Spectroscopy

Trupti Bhandari,* Dr.Alisha Patel, Khyati Dhodi, Zalak Desai, Saloni Desai
Department of Pharmaceutical Quality Assurance, ROFEL Shri G. M. Bilakhia College of Pharmacy, Vapi, India.
*Corresponding author’s E-mail: truptibhandari10897@gmail.com

Received: 05-09-2019; Revised: 23-10-2019; Accepted: 29-10-2019.

ABSTRACT
This experiment is used for the determination for to estimate the concentration of methyl paraben in cosmetics. Methyl paraben is
an antimicrobial agent, preservative, flavouring agent. The European Economic Community (EEC) Directive stipulates that parabens
are permitted in a concentration of up to 0.8% in cosmetics, with a maximum concentration for each individual one of 0.4% (w/w),
expressed as p-hyroxybenzoic acid. Effectively of parbens in high concentration causes cancer, genotoxicity and breast cancer.
Specifically for methyl paraben caused contact dermatitis and drug hypersensitivity. So, need to determine the concentration of
methyl paraben in cosmetics. The simple, rapid and sensitive UV spectroscopy method was developed for the determination of
methyl paraben in cosmetics products. Methyl paraben maximum absorbance at 254 nm. The extraction of Methyl paraben in
cosmetics may used cream, shampoo and lotion the optimal extraction solvent is methanol. The validation parameter of Methyl
paraben studied the Y= 0.081x+ 0.011, R2 = 0.9940. LOD and LOQ were 0.3095 and 0.9378.
Keywords: Methyl paraben, UV spectroscopy, cosmetics, validation.

INTRODUCTION stipulates that parabens are permitted in a concentration

of up to 0.8% in cosmetics, with a maximum concentration

M ethyl paraben other name is a 4-

hydroxybenzoate (methyl 4-hydroxybenzoate).1
It is the most frequently used antimicrobial
preservative in cosmetics and flavouring agent. .
Methylparaben is found in alcoholic beverages.
for each individual one of 0.4% (w/w), expressed as p-
hyroxybenzoic acid.3 Personal care product, such as hand
cream, facial cleanser and moisturizer, are widely used in
people’s daily lives. But parabens may be added into these
products during the production. It can be absorbed
Methylparaben odourless, small colourless crystals or
through the skin into the body.6 Antimicrobial
white crystalline powder Freely soluble in
effectiveness must be demonstrated for all products for all
alcohol, methanol, acetone, ether.Error! Reference source not found.
products contain antimicrobial preservatives and for
Instance paraben is now used for preservatives in food,
multiple dose topical dosage form and that is because the
pharmaceuticals and cosmetics, daily used the products
concentration of an antimicrobial preservatives may
that continue of methyl paraben may be caused in the
diminish during the shelf life of the product. Therefore the
future breast cancer.3 The super scale use of preservatives
concentration of preservative agents must be determent
in cosmetics can result in potential health risked. Most of
as well as the probable consumption of these agents
the preservatives may be harmful to the consumer due to
during the opening and closing of the cream must be
their potency to induce allergic contact dermatitis.4 Due to
calculated.7 Bacterial contamination of the products
their broad antimicrobial spectra with relatively low
through consumers use has resulted in presence of mixed
toxicity, good stability and non-voltality, parabens are
and harmful microbial flora in the product.8 Methyl
commonly used as preservatives to prevent alteration and
paraben is an antifungal and preservative that is widely
degradation of cosmetics, pharmaceutical and food from
used in cosmetics. Because it is easily absorbed through
microbial and fungal contamination and protect the
the skin and is generally considered non-irritating, it is a
consumers.4 Several of the parabens with reported uses
very popular beauty product ingredient and is used to
are used in products that can be ingested incidentally (e.g.,
prevent fungal growth and to generally preserve
Methyl paraben at up to 0.35% in lipstick), used near the
formulas.9 Despite their benefits, a controversy surrounds
eye (e.g., Methyl paraben at up to 0.8% in mascara), come
the discussion the effect of commonly used parabens,
in contact with mucous membranes (e.g., Methyl paraben
Methyl paraben, which can cause side effects on
at up to 0.5% in bath oils, tablets and salts), or in baby
consumers and organoleptics alterations in the cosmetics.
products (e.g., Methyl paraben at up to 0.4% in baby
The studies revealed that the use of parabens may cause
lotions, oils and creams).5 Hygienic standard for cosmetics
cancer, genotoxicity and breast cancer. Parabens are also
(2007 Edition, China) restricts the parabens preservatives
reported to have side effect on males as it may decrease
limited dose. The upper limit of mass percentages of single
the reproduction potential, cause infertility and cause
ester was 0.4% and the upper limit of mixed esters was
skin cancer diseases such as malignant, melanoma and
0.8%.6 The European Economic Community (EEC) Directive
contact eczema.10

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Int. J. Pharm. Sci. Rev. Res., 59(1), November - December 2019; Article No. 04, Pages: 17-21 ISSN 0976 – 044X

assurance that a specific process will consistently produce

a desired product meeting its predetermined
specifications and quality attributes.
Linearity (n=5)
The solution was prepared by pipetting 0.2, 0.4, 0.6, 0.8,
Figure 1: Methyl paraben and 1 ml from working stock solution into 10ml volumetric
flask and the volume was adjusted to mark with methanol
MATERIALS AND METHODS to produce 2-10μg/ml respectively. The absorbance of
Instrumentation solutions was measured at 254 nm. Calibration curve was
generated by taking the absorbance verses concentration.
UV-Visible spectrophotometer (Double beam) having two (Fig. 2,3 and Table 1)
matched quartz cells of light path 1 cm. shimadzu (UV-
1800). Electronic analytical weighing balance (REPTECH), Precision
Ultrasonicator (LOBA life). Repeatability (n=6)
Material and Reagents Aliquots of 0.6 ml of working standard solution of Methyl
Methyl paraben (ozone international Mumbai), Methanol. paraben (100μg/ml) were transferred to 10ml volumetric
flask and volume was adjusted to methanol to get
Method Preparation of Standard and Sample Solution concentration of 6μg/ml. The absorbance of solution was
Stock solution measured spectrophotometry six times and % RSD was
calculated. (Table no. 2)
100mg methyl paraben accurately weighed and
transferred into a 100ml volumetric flask and diluted up to Intraday precision (n=3)
the mark with methanol (1000ppm). Further 10 ml from Aliquots of 0.4, 0.6 and 0.8ml of working standard solution
methyl paraben stock solution was transferred into a 100 of Methyl paraben (100μg/ml) were transferred to 10ml
ml volumetric flask and diluted up to the mark with volumetric flask and volume was adjusted to methanol to
methanol (100ppm), then a series of solutions were get concentration of 4, 6 and 8μg/ml. The absorbance of
prepared by 2,4,6,8,10 ppm of diluted solution in to 10 ml solution was measured spectrophotometry three times
flasks and diluted up to the mark with methanol. and % RSD was calculated. For intraday, the analysis was
Sample (cream, lotion, shampoo) solution carried out at different intervals on the same day. (Table
no. 3)
The tested cosmetic products, including shampoo, body
lotion body creams, sun creams, face creams, make up Interday precision (n=3)
removals, were obtained at local markets. A 5.0 ml volume Aliquots of 0.4, 0.6 and 0.8ml of working standard solution
of methanol was added to the cosmetic samples (0.50gm). of Methyl paraben (100μg/ml) were transferred to 10ml
The emulsions were sonicated for 10 min, diluted to 10 ml volumetric flask and volume was adjusted to methanol to
and filtered through 0.22 µm Milipore membrane filters.6 get concentration of 4, 6 and 8μg/ml. The absorbance of
List of Cosmetic Products: solution was measured spectrophotometry three times on
the different days and % RSD was calculated. (Table no.4)
1. Alograce cream
Limit of detection (LOD)
2. Lakme cream
The LOD is estimated from the set of 3 calibration curves
3. Ponds cream used to determine method linearity. The LOD may be
4. Nivea cream calculated as,
5. Vaseline lotion LOD = 3.3 × (S.D./Slope)
6. Neem Aloevera face pack Where, SD = the standard deviation of Y- intercept of 3
calibration curves.
7. Dove shampoo
Slope = Mean slope of the 5 calibration curves.
8. Clinic plus shampoo
LOD= 0.3095004
9. Pantene shampoo
Limit of Quantitation (LOQ)
10. Almond shampoo
The LOD is estimated from the set of 3 calibration curves
Method Validation15,16 used to determine method linearity. The LOD may be
The method was validated according to ICH Q2 (R1) calculated as,
Guideline. Validation is a process of establishing LOQ = 10 × (S.D./Slope)
documented evidence, which provides degree of

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Int. J. Pharm. Sci. Rev. Res., 59(1), November - December 2019; Article No. 04, Pages: 17-21 ISSN 0976 – 044X

Where, SD= the standard deviation Methyl paraben in range 0.04 - 0.07% w/w in shampoos
which may be considered as safer for daily use. (Table 6).
Y= intercept of 3 calibration curves
1.000

Slope = Mean slope of the 3 calibration curves.

LOQ = O.93788 0.800

Robustness
0.600
Robustness of a method is a study of the effect of small

Abs.
variation of the experimental conditions on reproducibility
of the measurements. In the present investigation a study 0.400

of robustness was carried out by making a small change in

wavelength (±2) of measurements. (Table no.5) 0.200

Calculation
0.000
Concentration of methyl paraben 200.00 250.00 300.00 350.00 400.00
nm.

IN PPM (µg/ml): Figure 2: Linearity of Methyl paraben

Y= mx+c
Y = 0.081x+0.011 put the value of y= absorbance of sample
in this formula.
The value obtained x is your concentration in ppm (µg/ml)
IN MILIGRAM (mg)
Conc. Of methyl paraben (mg) = Concentration in ppm*
dilution factor
Here, dilution factor: 10/1*10/1*10/1 (1000) or,
10/1*10/1(100)
RESULTS AND DISCUSSION
Table 1: Linearity study of Methyl paraben

Concentration (µg/ml) Absorbance (254nm) Figure 3: Calibration curve of Methyl paraben.

2 0.1893 Table 2: Repeatability

4 0.3194
Sr. No. Absorbance
6 0.4823
1 0.4823
8 0.6887
2 0.4802
10 0.8177
3 0.4828
In most of selected cosmetics products the contents of 4 0.4822
Methyl paraben were found to be within specified range
5 0.4835
i.e. Not more than 0.4 % w/w. The products like Aloe grace
(0.420), Lakme (0.4064), Ponds (0.479), Vaseline (0.4041) 6 0.4932
shows content of Methyl paraben more than 0.4 % w/w MEAN 0.484033
and Aloe vera (0.1528) which contain amount less than
0.4% w/w and other products persist negligible amount of SD 0.004624
%RSD 0.955246

Table 3: Intraday precision

Sr. No. Conc.(µg/ml) Abs 1 Abs 2 Abs 3 Mean SD %RSD

1 4 0.3194 0.3261 0.3245 0.3233 0.0034 1.0821
2 6 0.4823 0.4891 0.4923 0.4879 0.0051 1.0467
3 8 0.6889 0.6811 0.6959 0.6886 0.0074 1.0751

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Int. J. Pharm. Sci. Rev. Res., 59(1), November - December 2019; Article No. 04, Pages: 17-21 ISSN 0976 – 044X

Table 4: Interday precision

Sr. No. Conc.(µg/ml) Abs 1 Abs 2 Abs 3 Mean SD %RSD

1 4 0.3194 0.3251 0.3295 0.3246 0.0050 1.5597
2 6 0.4823 0.4821 0.4933 0.4892 0.0060 1.2334
3 8 0.6889 0.6801 0.6989 0.6893 0.0094 1.3626

Table 5: Robustness
Wavelength (nm) Absorbance
252 0.4951
254 0.4823
256 0.4745

Table 6: Absorbance and % of Methyl paraben found in cosmetic products

Sr. No. Cosmetic product Absorbance % of methyl paraben found

1 Alograce cream 0.1815 0.4200
2 Lakme cream 0.1756 0.4064
3 Ponds cream 0.2050 0.4790
4 Nivea cream 0.1919 0.0440
5 Vaseline lotion 0.1747 0.4041
6 Neem aloe vera face pack 0.6302 0.1528
7 Dove shampoo 0.2034 0.0475
8 Clinic plus shampoo 0.3048 0.0725
9 Pantene shampoo 0.2181 0.0511
10 Almond shampoo 0.3048 0.0475

CONCLUSION 4. Manuela M. Mincea, Ioana R. Lupsa et al., “Determination

of Methylparaben from cosmetics products by ultra
The method of detected and validated parabens in daily performance liquid chromatography.” Journal of the
cosmetics by UV- spectroscopy was established. The result Serbian chemical society, 74(6), 2009, 669-676.
obtained confirm that the proposed method is simple,
5. The 2018 Cosmetic Ingredient Review Expert Panel
rapid, selective and a good sensitivity, for the
members are: Chair, Wilma F. Bergfeld, M.D., F.A.C.P.;
determination of Methyl paraben. Which did not need any Donald V. Belsito, M.D.; Ronald A. Hill, Ph.D.; Curtis D.
complex extraction procedure. The method of Klaassen, Ph.D.; Daniel C. Liebler, Ph.D.; James G. Marks, Jr.,
spectroscopy which shows maximum absorption at 254 nm. M.D.; Ronald C. Shank, Ph.D.; Thomas J. Slaga, Ph.D, and
It can be applied successfully for determination of methyl Paul W. Snyder, D.V.M., Ph.D. The CIR Executive Director is
paraben from cosmetic in range of 0.4 %. So, it is suitable Bart Heldreth, Ph.D. This report was prepared by Lillian C.
for the analysis of parabens in daily cosmetics. Becker, Scientific Analyst/Writer and Bart Heldreth. Safety
Assessment of parabens as Used in Cosmetics.
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Source of Support: Nil, Conflict of Interest: None.

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