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http://dx.doi.org/10.5806/AST.2020.33.3.125

Screening and detection of methylisothiazolinone and chloromethylisothiazolinone in cosmetics by UPLC-MS/MS  

Lee, Ji Hyun (Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Paek, Ji Hyun (Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Park, Han Na (Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Park, Seongsoo (Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Kang, Hoil (Division of Advanced Analysis, Toxicological Evaluation and Research Department, National Institute of Food and Drug Safety Evaluation, Ministry of Food and Drug Safety)
Publication Information
Analytical Science and Technology / v.33, no.3, 2020 , pp. 125-133 More about this Journal
Abstract
Methylisothiazolinone (MIT) and chloromethylisothiazolinone (CMIT) cause allergic contact dermatitis and are banned cosmetics ingredients, except in rinse-off products. However, their presence has been detected in cosmetics. We report a UPLC-tandem MS/MS screening method for their simultaneous determination in cosmetics. To facilitate extraction from various matrices, pretreatment methods were developed for each sample type. The method was optimized through a series of assessments, including specificity, LOD, LOQ, linearity, recovery, stability, precision, and accuracy. The LODs and LOQs for MIT ranged from 0.054 and 0.163 ㎍ mL-1 whereas those for CMIT ranged from 0.040 and 0.119 ㎍ mL-1. The linear correlation coefficients (r2) were higher than 0.999. Relative standard deviations (RSDs) for both intra- and inter-day measurements ranged from 0.3 ~ 13.6 %. Recoveries at three different concentrations were within 87.9 ~ 118.9 %. The RSD for stability measurements of spiked samples was within 7 %. These results confirm the suitability of the developed method for the simultaneous quantitation of MIT and CMIT in cosmetics. Samples of 320 color cosmetics, including eyeshadows, solid lipsticks, liquid lipsticks, and nail polishes were analyzed using the developed method, and two of them were found to contain both MIT and CMIT and one of them was found to contain only MIT. This data and the method will aid the regulation of ingredients used in cosmetics.
Keywords
LC-MS/MS; methylisothiazolinone; chloromethylisothiazolinone; cosmetics; screening;
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