Skip to main content
Log in

Vortex-assisted emulsification semimicroextraction for the analytical control of restricted ingredients in cosmetic products: determination of bronopol by liquid chromatography

  • Research Paper
  • Published:
Analytical and Bioanalytical Chemistry Aims and scope Submit manuscript

Abstract

Vortex-assisted emulsification semimicroextraction is proposed as a one-step solution-extraction procedure for sample preparation in cosmetic products. The procedure allows rapid preparation based on dispersion of the sample in a mixture of 1 mL of n-hexane and 0.5 mL of ethanol, followed by the addition of 0.5 mL of water and centrifugation to obtain two separated phases. This procedure provides good sample clean-up with minimum dilution and is very useful for the determination of ingredients with restricted concentrations, such as bronopol. The procedure was applied to the determination of bronopol by liquid chromatography with UV detection. The best chromatographic separation was obtained by using a C18 column set at 40 °C and performing a stepwise elution with a mixture of ethanol/aqueous 1 % acetic acid solution as mobile phase pumped at 0.5 mL min−1. The detection wavelength was set at 250 nm and the total run time required was 12 min. The method was successfully applied to 18 commercial cosmetic samples including creams, shampoos, and bath gels. Good recoveries and repeatability were obtained, with a limit of detection of 0.9 μg mL−1, which makes the method suitable for the analytical control of cosmetic products. Moreover, it could be considered environmentally friendly, because water, ethanol, and only a low volume of n-hexane are used as solvents.

Vortex-assisted emulsification semimicroextraction (VAEsME) for the preparation of cosmetic samples

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

References

  1. Regulation (EC) No. 1233/2009 of the European Parliament and of the Council of 30 November 2009 on cosmetic products. Annexes from III to VII.

  2. Salvador A, Chisvert A. An environmentally friendly (“green”) reversed-phase liquid chromatography method for UV filters determination in cosmetics. Anal Chim Acta. 2005;537:15–24.

    Article  CAS  Google Scholar 

  3. Chisvert A, Tarazona I, Salvador A. A reliable and environmentally-friendly liquid-chromatographic method for multi-class determination of fat-soluble UV filters in cosmetic products. Anal Chim Acta. 2013;790:61–7.

    Article  CAS  Google Scholar 

  4. Bryce DM, Croshaw B, Hall JE, Holland VR, Lessel B. The activity and safety of the antimicrobial agent bronopol (2-bromo-2-nitropropan-1,3-diol). J Soc Cosmet Chem. 1978;29:3–24.

    CAS  Google Scholar 

  5. Shepherd JA, Waigh RD, Gilbert P. Antibacterial action of 2-bromo-2-nitropropane-1,3-diol (bronopol). Antimicrob Agents Chemother. 1988;32:1693–8.

    Article  CAS  Google Scholar 

  6. Commission Regulation (EU) No. 358/2014 of 9 April 2014 amending Annexes II and V to Regulation (EC) No. 1233/2009 of the European Parliament and of the Council of 30 November 2009 on cosmetic products.

  7. Matczuk M, Obarski N, Mojski M. The impact of the various chemical and physical factors on the degradation rate of bronopol. Int J Cosmet Sci. 2012;34:451–7.

    Article  CAS  Google Scholar 

  8. Kajimura K, Tagami T, Yamamoto T, Iwagami S. The release of formaldehyde upon decomposition of 2-bromo-2-nitropropane-1,3-diol (bronopol). J Health Sci. 2008;54:488–92.

    Article  CAS  Google Scholar 

  9. Cui N, Zhang X, Xie Q, Wang S, Chen J, Huang L, et al. Toxicity profile of labile preservative bronopol in water: the role of more persistent and toxic transformation products. Environ Pollut. 2011;159:609–15.

    Article  CAS  Google Scholar 

  10. SCCS (Scientific Committee on Consumer Safety) (2012) Opinion on nitrosamines and secondary amines in cosmetic products.

  11. Ferioli V, Vezzalini F, Rustichelli C, Gambernini G. Determination of bronidox and bronopol in cosmetic products by reversed phase high-performance liquid chromatography. Farmaco. 1992;47:833–9.

    CAS  Google Scholar 

  12. Hu J, Wang J. Determination of eleven preservatives including bronopol in cosmetic by reversed-phase ion-pair chromatography. Chin J Chromatogr. 1999;17:495–7.

    CAS  Google Scholar 

  13. Wang HF, Provan GJ, Helliwell K. Determination of bronopol and its degradation products by HPLC. J Pharm Biomed. 2002;29:387–92.

    Article  CAS  Google Scholar 

  14. Marengo E, Gianotti V, Angioi S, Gennaro MC. Optimization by experimental design and artificial neural networks of the ion-interaction reversed-phase liquid chromatographic separation of twenty cosmetic preservatives. J Chromatogr A. 2004;1029:57–65.

    Article  CAS  Google Scholar 

  15. Weyland JW, Stern A, Rooselaar J. Determination of bronopol, bronidox and methyldibromo glutaronitrile in cosmetics by liquid chromatography with electrochemical detection. J AOAC Int. 1994;77:1132–6.

    CAS  Google Scholar 

  16. Scalia S, Simeoni S, Bousquet E. Determination of bronopol in cosmetic products by HPLC with electrochemical detection. Pharmazie. 2001;56:318–20.

    CAS  Google Scholar 

  17. Bendahl L, Hansen SH, Gammergaard B, Sturup S, Nielsen C. Hyphenation of ultra performance liquid chromatography (UPLC) with inductively coupled plasma mass spectrometry (ICP-MS) for fast analysis of bromine containing preservatives. J Pharm Biomed. 2006;40:648–52.

    Article  CAS  Google Scholar 

  18. Wu T, Wang C, Wang X, Ma Q. Simultaneous determination of 21 preservatives in cosmetics by ultra performance liquid chromatography. Int J Cosmet Sci. 2006;30:367–72.

    Article  Google Scholar 

  19. Fernandez-Alvarez M, Lamas JP, Sanchez-Prado L, Llompart M, Garcia-Jares C, Lores M. Development of a solid-phase microextraction gas chromatography with microelectron-capture detection method for the determination of 5-bromo-5-nitro-1,3-dioxane in rinse-off cosmetics. J Chromatogr A. 2010;1217:6634–9.

    Article  CAS  Google Scholar 

  20. Yiantzi E, Psillakis E, Tyrovola K, Kalogerakis N. Vortex-assisted liquid-liquid microextraction of octylphenol, nonylphenol and bisphenol-A. Talanta. 2010;80:2057–62.

    Article  CAS  Google Scholar 

  21. Perez-Serradilla JA, Priego-Capote F, Luque de Castro JA. Simultaneous ultrasound-assisted emulsification–extraction of polar and nonpolar compounds from solid plant samples. Anal Chem. 2007;79:6767–74.

    Article  CAS  Google Scholar 

  22. Regueiro J, Llompart M, Garcia-Jares C, Garcia-Monteagudo JC, Cela R. Ultrasound-assisted emulsification-microextraction of emergent contaminants and pesticides in environmental waters. J Chromatogr A. 2008;1190:27–38.

    Article  CAS  Google Scholar 

  23. Regueiro J, Llompart M, Psillakis E, Garcia-Monteagudo JC, Garcia-Jares C. Ultrasound-assisted emulsification-microextraction of phenolic preservatives in water. Talanta. 2009;79:1387–97.

    Article  CAS  Google Scholar 

  24. Perez-Outeiral J, Millan E, Garcia-Arrona R. Ultrasound-assisted emulsification microextraction coupled with high-performance liquid chromatography for the simultaneous determination of fragrance allergens in cosmetics and water. J Sep Sci. 2015;38:1561–9.

    Article  CAS  Google Scholar 

  25. Gonzalez-Hernandez P, Pino V, Ayala JH, Afonso AM. A simplified vortex-assisted emulsification microextraction method for determining personal care products in environmental water samples by ultra-high-performance liquid chromatography. Anal Methods. 2015;7:1825–33.

    Article  CAS  Google Scholar 

  26. Jia C, Zhu X, Wang J, Zhao E, He M, Chen L, et al. Extraction of pesticides in water samples using vortex-assisted liquid-liquid microextraction. J Chromatogr A. 2010;1217:5868–71.

    Article  CAS  Google Scholar 

  27. Papadopoulou A, Roman IP, Canals A, Tyrovola K, Psillakis E. Fast screening of perfluorooctane sulfonate in water using vortex-assisted liquid-liquid microextraction coupled to liquid chromatography-mass spectrometry. Anal Chim Acta. 2011;691:56–61.

    Article  CAS  Google Scholar 

  28. Yang Z, Lu Y, Liu Y, Wu T, Zhou Z, Liu D. Vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction. J Chromatogr A. 2011;1218:7071–7.

    Article  CAS  Google Scholar 

  29. Moreno-Gonzalez D, Huertas-Perez JF, Garcia-Campana AM, Gamiz-Gracia L. Vortex-assisted surfactant-enhanced emulsification liquid-liquid microextraction for the determination of carbamates in juices by micellar electrokinetic chromatography tandem mass spectrometry. Talanta. 2015;139:174–80.

    Article  CAS  Google Scholar 

  30. Leng G, Chen W, Zhang M, Huang F, Cao Q. Determination of phthalate esters in liquor samples by vortex-assisted surfactant-enhanced-emulsification liquid-liquid microextraction followed by GC-MS. J Sep Sci. 2014;37:684–90.

    Article  CAS  Google Scholar 

  31. Andruch V, Burdel M, Kocurova L, Sandrejova J, Balogh IS. Application of ultrasonic irradiation and vortex agitation in solvent microextraction. Trends Anal Chem. 2013;49:1–19.

    Article  CAS  Google Scholar 

  32. Moradi M, Yamini Y, Ebrahimpour B. Emulsion-based liquid-phase microextraction: a review. J Iran Chem Soc. 2014;11:1087–101.

    Article  Google Scholar 

  33. Spietelun A, Marcinkowski L, de la Guardia M, Namiesnik J. Green aspects, developments and perspectives of liquid phase microextraction techniques. Talanta. 2014;119:34–45.

    Article  CAS  Google Scholar 

  34. Miralles P, Chisvert A, Salvador A. Determination of hydroxytyrosol and tyrosol by liquid chromatography for the quality control of cosmetic products based on olive extracts. J Pharm Biomed. 2015;102:157–61.

    Article  CAS  Google Scholar 

Download references

Acknowledgments

P.M. would like to thank the Spanish ‘Ministerio de Educación, Cultura y Deporte’ for his predoctoral grant.

Author information

Authors and Affiliations

Authors

Corresponding author

Correspondence to Amparo Salvador.

Ethics declarations

We wish to confirm that there are no known conflicts of interest associated with this publication and there has been no financial support for this work that could have influenced its outcome.

Rights and permissions

Reprints and permissions

About this article

Check for updates. Verify currency and authenticity via CrossMark

Cite this article

Miralles, P., Bellver, R., Chisvert, A. et al. Vortex-assisted emulsification semimicroextraction for the analytical control of restricted ingredients in cosmetic products: determination of bronopol by liquid chromatography. Anal Bioanal Chem 408, 1929–1934 (2016). https://doi.org/10.1007/s00216-016-9306-5

Download citation

  • Received:

  • Revised:

  • Accepted:

  • Published:

  • Issue Date:

  • DOI: https://doi.org/10.1007/s00216-016-9306-5

Keywords

Navigation