Skip to main content
Log in

Development and validation of a new method for determination of methylparaben in Iran market infant formulae by HPLC

  • Research article
  • Published:
Journal of Environmental Health Science and Engineering Aims and scope Submit manuscript

Abstract

Background

Parabens are esters of p-hydroxybenzoic acid and are widely used as preservatives in cosmetics, pharmaceuticals and foodstuffs. The presences of parabens in infant formulas raise concerns due to their potential to disrupt endocrine function in infants and cause reproductive toxicities.

Methods

In this study a new method was developed for extraction and determination of methylparaben in infant formulas using HPLC method and UV detector. Methanol and trichloroacetic acid were used for extraction and isocratic mobile phase comprising equal proportions of glacial acetic acid in water (50:850 v/v) and methanol was used for separation of methylparaben.

Results

Recovery of the extraction procedure was good and interferences between methylparaben and other ingredients peaks in HPLC chromatograms decreased. The average recoveries for methylparaben were about 88–108 %. The limit of detection and limit of quantitation for methylparaben were 0.2 and 0.5 µg/mL, respectively. Results of the method showed good reproducibility (relative standard deviation (RSD) 0.29–1.94 % for within day analysis and 0.84–2.18 % for between day analysis). Results were linear in range of 0.5–20 µg/mL methylparaben. The results of twenty real infant formula samples showed methylparaben was found only in one sample in concentration 0.3 µg/mL.

Conclusions

The new extraction and measurement method was a short-time method and could be applicable for large numbers of samples. This method was fast, sensitive and accurate and was capable of being used in legal laboratory references for determination of methylparaben content.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Fig. 1
Fig. 2

Similar content being viewed by others

Data availability

The data will not be shared with a reason.

Code availability

Not applicable.

References

  1. Rastogi SC, Schouten A, De Kruijf N, Weijland JW. Contents of methyl-, ethyl-, propyl-, butyl- and benzylparaben in cosmetic products. Contact Dermatitis. 1995;32(1):28–30.

    Article  CAS  Google Scholar 

  2. Soni MG, Taylor SL, Greenberg NA, Burdock GA. Evaluation of the health aspects of methyl paraben: a review of the published literature. Food Chem Toxicol. 2002;40(10):1335–73.

    Article  CAS  Google Scholar 

  3. Soni MG, Carabin IG, Burdock GA. Safety assessment of esters of p-hydroxybenzoic acid (parabens). Food Chem Toxicol. 2005;43(7):985–1015.

    Article  CAS  Google Scholar 

  4. Zhang Q, Lian M, Liu L, Cui H. High-performance liquid chromatographic assay of parabens in wash-off cosmetic products and foods using chemiluminescence detection. Anal Chim Acta. 2005;537(1):31–9.

    Article  CAS  Google Scholar 

  5. Andersen FA. Final amended report on the safety assessment of methylparaben, ethylparaben, propylparaben, isopropylparaben, butylparaben, isobutylparaben, and benzylparaben as used in cosmetic products. Int J Toxicol. 2008;27(Suppl 4):1–82.

    Google Scholar 

  6. Eriksson E, Andersen HR, Ledin A. Substance flow analysis of parabens in Denmark complemented with a survey of presence and frequency in various commodities. J Hazard Mater. 2008;156(1–3):240–59.

    Article  CAS  Google Scholar 

  7. El Hussein S, Muret P, Berard M, Makki S, Humbert P. Assessment of principal parabens used in cosmetics after their passage through human epidermis-dermis layers (ex-vivo study). Exp Dermatol. 2007;16(10):830–6.

    Article  Google Scholar 

  8. Ye X, Kuklenyik Z, Bishop AM, Needham LL, Calafat AM. Quantification of the urinary concentrations of parabens in humans by on-line solid phase extraction-high performance liquid chromatography-isotope dilution tandem mass spectrometry. J Chromatogr B Analyt Technol Biomed Life Sci. 2006;844(1):53–9.

    Article  CAS  Google Scholar 

  9. Ye X, Bishop AM, Reidy JA, Needham LL, Calafat AM. Parabens as urinary biomarkers of exposure in humans. Environ Health Perspect. 2006;114(12):1843–6.

    Article  CAS  Google Scholar 

  10. Ye X, Tao LJ, Needham LL, Calafat AM. Automated on-line column-switching HPLC-MS/MS method for measuring environmental phenols and parabens in serum. Talanta. 2008;76(4):865–71.

    Article  CAS  Google Scholar 

  11. Calafat AM, Ye X, Wong LY, Bishop AM, Needham LL. Urinary concentrations of four parabens in the U.S. population: NHANES 2005–2006. Environ Health Perspect. 2010;118(5):679–85.

    Article  CAS  Google Scholar 

  12. Schlumpf M, Kypke K, Wittassek M, Angerer J, Mascher H, Mascher D, et al. Exposure patterns of UV filters, fragrances, parabens, phthalates, organochlor pesticides, PBDEs, and PCBs in human milk: correlation of UV filters with use of cosmetics. Chemosphere. 2010;81(10):1171–83.

    Article  CAS  Google Scholar 

  13. Casas L, Fernandez MF, Llop S, Guxens M, Ballester F, Olea N, et al. Urinary concentrations of phthalates and phenols in a population of Spanish pregnant women and children. Environ Int. 2011;37(5):858–66.

    Article  CAS  Google Scholar 

  14. Frederiksen H, Jorgensen N, Andersson AM. Parabens in urine, serum and seminal plasma from healthy Danish men determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS). J Expo Sci Environ Epidemiol. 2011;21(3):262–71.

    Article  CAS  Google Scholar 

  15. Smith KW, Braun JM, Williams PL, Ehrlich S, Correia KF, Calafat AM, et al. Predictors and variability of urinary paraben concentrations in men and women, including before and during pregnancy. Environ Health Perspect. 2012;120(11):1538–43.

    Article  CAS  Google Scholar 

  16. Miller D, Wheals BB, Beresford N, Sumpter JP. Estrogenic activity of phenolic additives determined by an in vitro yeast bioassay. Environmental health perspectives. 2001;109(2):133–8.

    Article  CAS  Google Scholar 

  17. Okubo T, Yokoyama Y, Kano K, Kano I. ER-dependent estrogenic activity of parabens assessed by proliferation of human breast cancer MCF-7 cells and expression of ERalpha and PR. Food Chem Toxicol. 2001;39(12):1225–32.

    Article  CAS  Google Scholar 

  18. Byford JR, Shaw LE, Drew MG, Pope GS, Sauer MJ, Darbre PD. Oestrogenic activity of parabens in MCF7 human breast cancer cells. J Steroid Biochem Mol Biol. 2002;80(1):49–60.

    Article  CAS  Google Scholar 

  19. Darbre PD, Harvey PW. Paraben esters: review of recent studies of endocrine toxicity, absorption, esterase and human exposure, and discussion of potential human health risks. J Appl Toxicol. 2008;28(5):561–78.

    Article  CAS  Google Scholar 

  20. Boberg J, Taxvig C, Christiansen S, Hass U. Possible endocrine disrupting effects of parabens and their metabolites. Reprod Toxicol. 2010;30(2):301–12.

    Article  CAS  Google Scholar 

  21. Witorsch RJ, Thomas JA. Personal care products and endocrine disruption: a critical review of the literature. Crit Rev Toxicol. 2010;40(Suppl 3):1–30.

    Article  CAS  Google Scholar 

  22. Routledge EJ, Parker J, Odum J, Ashby J, Sumpter JP. Some alkyl hydroxy benzoate preservatives (parabens) are estrogenic. Toxicol Appl Pharmacol. 1998;153(1):12–9.

    Article  CAS  Google Scholar 

  23. Pedersen KL, Pedersen SN, Christiansen LB, Korsgaard B, Bjerregaard P. The preservatives ethyl-, propyl- and butylparaben are oestrogenic in an in vivo fish assay. Pharmacol Toxicol. 2000;86(3):110–3.

    Article  CAS  Google Scholar 

  24. Oishi S. Effects of propyl paraben on the male reproductive system. Food Chem Toxicol. 2002;40(12):1807–13.

    Article  CAS  Google Scholar 

  25. Oishi S. Effects of butyl paraben on the male reproductive system in mice. Arch Toxicol. 2002;76(7):423–9.

    Article  CAS  Google Scholar 

  26. Toxicological evaluation of certain food additives with a review of general principles and of specifications. Seventeenth report of the joint FAO-WHO Expert Committee on Food Additives. 1974/01/01 ed1974. 1–40 p.

  27. Scientific committee on consumer safety. SCCS/1446/11 Clarification on Opinion SCCS/1348/10 in the light of the Danish clause of safeguard banning the use of parabens in cosmetic products intended for children under three years of age. 10 October 2011.

  28. Liao C, Liu F, Kannan K. Occurrence of and dietary exposure to parabens in foodstuffs from the United States. Environ Sci Technol. 2013;47(8):3918–25.

    Article  CAS  Google Scholar 

  29. Martin CR, Ling P-R, Blackburn GL. Review of infant feeding: key features of breast milk and infant formula. Nutrients. 2016;8(5):279.

    Article  Google Scholar 

  30. Lemaire M, Le Huërou-Luron I, Blat S. Effects of infant formula composition on long-term metabolic health. J Dev Orig Health Dis. 2018;9(6):573–89.

    Article  CAS  Google Scholar 

  31. Wu H, Wu L-H, Wang F, Gao C-J, Chen D, Guo Y. Several environmental endocrine disruptors in beverages from South China: occurrence and human exposure. Environ Sci Pollut Res Int. 2019;26(6):5873–84.

    Article  CAS  Google Scholar 

  32. Chiesa LM, Pavlovic R, Panseri S, Arioli F. Evaluation of parabens and their metabolites in fish and fish products: a comprehensive analytical approach using LC-HRMS. Food Addit Contam Part A Chem Anal Control Expo Risk Assess. 2018;35(12):2400–13.

    Article  CAS  Google Scholar 

  33. Del Olmo A, Calzada J, Nuñez M. Benzoic acid and its derivatives as naturally occurring compounds in foods and as additives: Uses, exposure, and controversy. Crit Rev Food Sci Nutr. 2017;57(14):3084–103.

    Article  Google Scholar 

  34. Gao Y, Wang Y, Yan Y, Tang K, Ding CF. Self-assembly of poly(ionic liquid) functionalized mesoporous magnetic microspheres for the solid-phase extraction of preservatives from milk samples. J Sep Sci. 2020;43(4):766–73.

    Article  CAS  Google Scholar 

  35. Sivaraman T, Kumar TK, Jayaraman G, Yu C. The mechanism of 2,2,2-trichloroacetic acid-induced protein precipitation. J Protein Chem. 1997;16(4):291–7.

    Article  CAS  Google Scholar 

Download references

Acknowledgements

We are grateful Food and Drug Control Reference Laboratory, Iranian Food and Drug Administration for their assistance and providing some reagents.

Funding

The research was conducted with the internal funding of the Food and Drug Laboratory Research Center, Food and Drug Administration and no grants were used.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Roya Khosrokhavar.

Ethics declarations

Conflict of interest

All authors declare that they have no conflict of interest.

Ethical approval

This article does not contain any studies with human or animals.

Additional information

Publisher’s note

Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Khansari, N., Adib, N., Alikhani, A. et al. Development and validation of a new method for determination of methylparaben in Iran market infant formulae by HPLC. J Environ Health Sci Engineer 19, 565–572 (2021). https://doi.org/10.1007/s40201-021-00628-7

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s40201-021-00628-7

Keywords

Navigation