超高效液相色谱-串联质谱法同时测定化妆品中50种非法添加药物

建立超高效液相色谱-串联质谱(UPLC-MS/MS)同时测定化妆品中50种非法添加化学药物定性筛查及定量分析方法.不同基质样品经乙腈溶液(含0.5%甲酸)提取后,冷冻离心,上清液采用2 mg/L乙二胺四乙酸二钠水溶液定容,以甲醇-0.1%甲酸溶液为流动相,经CAPCELL CORE C18色谱柱梯度洗脱分离.采用电喷雾电离(ESI),以多重反应监测(MRM)模式进行正负离子检测.所测50种化学药物在10~100 ng/mL范围内呈现良好的线性关系(r值均大于0.991 0),精密度、重复性良好,平均回收率在87.2%~109.7%之间,相对标准偏差(RSD)不超过10.0%,方法检出限为0.05~33 ng/g,定量限为0.15~99 ng/g.方法简便、灵敏度高、重复性好,可以实现化妆品中50种非法添加化学药物快速、准确的定性筛查和定量测定.

Simultaneous Determination of 50 Prohibited Drugs in Cosmetics by Ultra-High Performance Liquid Chromatography Tandem Mass Spectrometry

A method for the quantitative analysis of 50 prohibited drugs in cosmetics by ultra-high performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS) has been developed. The samples were extracted with acetonitrile (containing 0.5% formic acid) by ultrasonic extraction, freezing centrifuged, and the supernatant was fixed in an ethylenediaminetetraacetic acid disodium salt solution (2 mg/L). Then the analytes were separated using a CAPCELL CORE C18 chromatographic column with mobile phase A (methanol) and mobile phase B (0.1% formic acid in water) by gradient elution, finally analyzed by positive and negative mode with electrospray ion source (ESI). The data were acquired by a multiple reactions monitoring (MRM) mode. In the mass concentration range of 10~100 ng/mL, 50 prohibited drugs showed good linear relationship with all their correlation coefficients (r) more than 0.991 0. The detection limits were within 0.05~33 ng/g, and the quantification limits were within 0.15~99 ng/g. The average recovery rates of the samples were within 87.2%~109.7% with the relative standard deviations（RSD) not greater than 10.0%. The method is simple, sensitive and reproducible, and can be used for the rapid and accurate qualitative screening and quantitative determination of 50 prohibited drugs in cosmetics.