化妆品中氯胺T的超声辅助水解/液相色谱检测及质谱确证

Determination of Chloramine T in Cosmetics by Ultrasound-assisted Hydrolyzation-LC and Validation by LC-MS/MS

建立了化妆品中氯胺T的超声辅助水解/高效液相色谱分析方法,并采用液相色谱-串联质谱进行确证。将不同类型(膏霜、水剂、散粉、香波、牙膏)化妆品样品分散于盐酸溶液中,超声波辅助提取并水解氯胺T,水解液用乙醚萃取后,采用高效液相色谱分离分析,以Agilent Extend C18(4.6 mm×250 mm,5μm)为色谱柱,乙腈-水为流动相,等度洗脱,二极管阵列检测器检测,外标法定量;采用液相色谱-串联质谱法进一步确证分析,Agilent Poroshell C18(4.6 mm×100 mm,2.7μm)色谱柱分离,电喷雾正离子模式电离,多反应监测模式检测。结果表明,该法对氯胺T的定量下限为16.5 mg/kg,线性范围为1.0～500.0 mg/L,相关系数(r2)为0.999 9。在低、中、高3种加标水平的回收率为81%～103%,相对标准偏差为1.0%～7.4%。该方法简便、快速、准确、灵敏,适用于化妆品中氯胺T的检测。

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 172.0491.10 and m/z 172.04155.02,in which m/z 172.0491.10 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.