An Ultrasound-assisted extraction and hydrolyzation plus high performance liquid chromatographic(HPLC) method was developed for the determination of chloramine T in cosmetics.A liquid chromatography-tandem mass spectrometric(LC-MS/MS) method was also established for the verification of the results.Different cosmetic products,e.g.cream,lotion,powder,shampoo and toothpaste, were extracted ultrasonically and hydrolyzed with hydrochloric acid solution.The hydrolyzate was isolated by liquid-liquid extraction with ethyl ether.The determination of chloramine T was performed by HPLC on an Agilent Extend C18 column(4.6 mm×250 mm,5μm) using acetonitrile-water as mobile phase at a detection wavelength of 224 nm, and quantified by the external standard method.The verification analysis was achieved by LC-MS/MS method on an Agilent Poroshell C18 column(4.6 mm×100 mm,2.7 μm),under positive electrospray ionization and multiple reactions monitoring(MRM) mode.For p toluenesulfonamide,the MS/MS detection transitions were m/z 172.04>91.10 and m/z 172.04>155.02,in which m/z 172.04>91.10 was used as the quantitative transition.Under the optimal conditions,the calibration curve was linear in the range of 1.0-500.0 mg/L,with correlation coefficient of 0.999 9.The limit of quantification(LOQ) was 16.5 mg/kg.The mean recoveries at three spiked levels were in the range of 81%-103%with RSDs of 1.0%-7.4%.The method was simple,rapid,accurate and sensitive,and was suitable for the determination of chloramine T in cosmetic samples.
关键词
液相色谱液相色谱-串联质谱超声辅助水解氯胺T对甲苯磺酰胺化妆品
Keywords
liquid chromatographyliquid chromatography-tandem mass spectrometryultrasound-assisted extraction and hydrolyzationchloramine Tp toluenesulfonamidecosmetics
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Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology,Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine,Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,),Guangzhou
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International Cooperation Joint Laboratory for Intelligent Preparation of High-end Functional Mineral Salt Materials,National & Local Joint Engineering Research Center for Mineral Salt Deep Utilization,Huaiyin Institute of Technology,Huai’an