대한화장품학회지 (Journal of the Society of Cosmetic Scientists of Korea)

  • 제48권4호
  • /
  • Pages.321-330
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  • 2022
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  • 1226-2587(pISSN)
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  • 2288-9507(eISSN)
대한화장품학회 (Society of Cosmetic Scientists of Korea)
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HPLC 를 이용한 화장품 중 살균보존제 다성분 동시분석법 연구

Analytical Method of Multi-Preservatives in Cosmetics using High Performance Liquid Chromatography

  • 투고 : 2022.10.14
  • 심사 : 2022.12.09
  • 발행 : 2022.12.30
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초록

본 연구는 HPLC-PDA를 이용하여 화장품의 보존제 15 종, 자외선 차단제 2종 및 항산화제 1 종에 대해 신뢰성 있는 결과를 확보할 수 있는 최적의 다성분 동시분석법을 구축하고자 하였다. 이동상의 수소이온 농도(pH)가 분석성분의 산해리상수(pKa)에 영향을 주기 때문에 피크의 머무름 시간과 면적값 변화가 생기는 문제를 확인하였고, 이동상 조제시 0.1% H3PO4 첨가량(mL)으로 pH를 조절하는 방법으로써 피크 분리조건을 확립하였다. 시험법의 유효성 검증 결과, 검량선의 직선성(R2)은 0.999 이상을 얻었으며 화장품 2 종(크림, 샴푸)에 대해 정확성은 87.9 ~ 101.1%, 정밀성은 0.1 ~ 7.6% 의 결과를 얻었다. 성분별로 검출한계(LOD)는 0.1 ~ 0.2 mg/kg, 정량한계(LOQ)는 2.0 ~ 4.0 mg/kg인 것으로 나타났다. 또한 합성보존제인 methylparaben과 차이점이 적어 HPLC에서 성분분리가 어려웠던 천연성분인 p-anisic acid를 동시에 분리할 수 있었다. 본 연구를 통해 화장품 중 사용상 제한이 필요한 성분들에 대한 품질관리 및 안전성 확보에 효과적으로 활용될 것이다.

This study attempted to establish an optimal multi-compound simultaneous analysis method that can secure reliable results for 15 - preservatives, 2 - sun screens and 1 - antioxidants of cosmetics using HPLC-PDA. Since the potential of hydrogen (pH) in the mobile phase affects the acid dissociation constant (pKa) of the preservatives, and the peak retention time shift and area change were observed. The peak separation condition was established by adjusting the pH to 0.1% H3PO4 addition (mL) when preparing the mobile phase. As a results of method validation, the linearity correlation coefficient (R2) of above 0.999 were obtained, and accuracy 87.9 ~ 101.1%, 0.1 ~ 7.6% precision for two types of cosmetics (cream and shampoo). It was found that the limit of detection (LOD) was 0.1 ~ 0.2 mg/kg and the limit of quantitation (LOQ) was 2.0 ~ 4.0 mg/kg. In addition, it was possible to simultaneously separate p-anisic acid, a natural compound that was difficult to separate in HPLC due to the small difference from methylparaben, a synthetic preservatives. Through this study, it will be effectively used to secure quality control and safety for compound that need restrictions on use cosmetics.

키워드

참고문헌

  1. K. H. Lee, Master's Thesis Dissertation, Chung-Ang Univ., Seoul, Korea (2010).
  2. E. J. Routledge, J. Parker, J. Odum, J. Ashby, and J. P. Sumpter, Some alkyl hydroxy benzoate preservatives (Parabens) are estrogenic, Toxicology and Applied Pharmacology, 153(1), 12 (1998).
  3. G. A. Shabir, Determination of combined p-hydroxy benzoic acid preservatives in a liquid pharmaceutical formulation by HPLC, J. Pharm. Biomed. Anal., 34(1), 207 (2004).
  4. J. E. Park, S. M. Lee, H. J. Jeong, and I. S. Chang, Simultaneous determination of 8 preservatives (6 parabens, 2-phenoxyethanol and chlorphenesin) in cosmetics by UPLCTM, J. Soc. Cosmet. Sci. Korea, 33(4), 263 (2007).
  5. J. S. Jeon, H. T. Kim, M. G. Kim, M. S. Oh, S. R. Hong, M. H. Yoon, S. M. Cho, H. C. Shin, J. H. Shim, A. Ramadan, and A. M. Abd El-Aty, Simultaneous determination of water-soluble whitening ingredients and adenosine in different cosmetic formulations by high-performance liquid chromatography coupled with photodiode array detection, Int. J. Cosmet. Sci., 38(3), 286 (2016).
  6. J. L. Olivelra Arlas, C. B. Rocha, A. L. Q. Silva Santos, L. C. Marube, L. Kupskl, S. S. Caldas, and E. G. Primel, Fast and simple method of simultaneous preservatives determination in different processed foods by QuEChERS and HPLC-UV : Method development, survey and estimate of daily intake, Food Chemistry, 293, 112 (2019).
  7. S. H. Cho, H. R. Jung, Y. S. Kim, Y. H. Kim, E. M. Park, S. W. Shin, K. S. Eum, S. R. Hong, H. J. Kang, and M. H. Yoon, Simultaneous multicomponent analysis of preservatives in cosmetics by gas chromatography, J. Soc. Cosmet. Sci. Korea, 45(1), 69 (2019).
  8. M. R. Lee, C. Y. Lin, Z. G. Li, and T. F. Tsai, Simultaneous analysis of antioxidants and preservatives in cosmetics by supercritical fluid extraction combined with liquid chromatography-mass spectrometry, J. Chromatogr. A, 1120(1-2), 244 (2006).
  9. M. Akkbik, Z. B Assim, and F. B. Ahmad, Optimization and validation of RP-HPLC-UV/Vis method for determination phenolic compounds in several personal care products, Int. J. Anal. Chem., 2011, 858153, https://doi.org/10.1155/2011/858153 (2011).
  10. S. J. Jung, Y. S. Hwang, C. M. Choi, A. S. Park, S. U. Kim, H. J Kim, J. H. Kim, and K. Jung, Examination and quantification of preservatives in cosmetics for chlidren, J. Soc. Cosmet. Sci. Korea, 41(3), 219 (2015).
  11. N. R. Cha, J. K. Lee, H. J. Jeong, J. C. Cho, M. J. Kim, and S. Y. Lee, Determination of 19 preservatives in various matrices by high-performance liquid chromatography, Analytical Letters, 45(15), 2148 (2012).
  12. R. Kaliszam, P. Wiczling, and J. Markuszewski, pH gradient high-performance liquid chromatography: theory and applications, J. Chromatogr. A, 1060(1-2), 165 (2004).
  13. W. Gao and C. Legido-Quigley, Fast and sensitive high performance liquid chromatography analysis of cosmetic creams for hydroquinone, phenol and six preservatives, J. Chromatogr. A, 1218(28), 4307 (2011).
  14. T. Wu, C. Wang, X. Wang, and Q. Ma, Simultaneous determination of 21 preservatives in cosmetics by ultra performance liquid chromatography, Int. J. Cosmet. Sci., 30(5), 367 (2008).
  15. I. Baranowska and I. Wojciechowska, The determination of preservatives in cosmetics and environmental waters by HPLC, Pol. J. Environ. Stud. 22(6), 1609 (2013).
  16. A. Kim, Y. J. Lee, Y. S. Cho, H. J. Kim, S. H. Cho, Y. H. Kim, J. W Ro, and Y. B. Park, A study on filters, preservatives and heavy metals contained in the children's and inorganic sunscreens distributed in Korea, J. Soc. Cosmet. Sci. Korea, 47(4), 289 (2021).
  17. I. H. Kim, D. H. Ryu, Y. S. Kim, E. S. Jung, and D. H. Park, Determination of p-anisic acid and methylparaben by using high performance liquid chromatography, J. Soc. Cosmet. Sci. Korea, 40(4), 359 (2014).
  18. G. Alvarez-Riverra, T. Dagnac, M. Lores, G. Garcia-Jares, L. Sanchez-Prado, J. Pablo Lamas, and M. Llompart, Determination of isothiazolinone preservatives in cosmetics and household products by matrix solid-phase dispersion followed by high-performance liquid chromatography-tandem mass spectrometry, J. Chromatogr. A, 1270, 41 (2012).