固相萃取-同位素稀释-气相色谱-串联质谱法测定化妆品中的二甲苯麝香

Determination of Musk Xylene in Cosmetics by Solid Phase Extraction-Isotope Dilution-Gas Chromatography Tandem Mass Spectrometry

建立了测定化妆品中二甲苯麝香的固相萃取-同位素稀释-气相色谱-串联质谱分析方法。膏霜、水剂、散粉、香波、唇膏等不同类型的化妆品样品加入甲醇经超声提取后,样品提取液高速离心处理,浓缩上清液,以Sep-Pak Silica固相萃取柱净化,收集二氯甲烷洗脱液,DB-5 MS(30 m×0.25 mm,0.25μm)石英毛细管色谱柱分离后经NCI-GC-MS/MS多反应监测技术进行定性及定量分析。二甲苯麝香的方法定量限为5μg/kg,在5～50μg/kg范围内的3个添加水平的平均回收率为81.1%～86.9%,日内精密度均小于10%,日间精密度均小于12%。本方法准确、快速、灵敏度高,可用于化妆品的实际检验工作。

A comprehensive analytical method based on solid phase extraction-isotope dilution-gas chromatog-raphy tandem mass spectrometry has been developed for the determination of musk xylene in cosmetics. Various cosmetic samples, including cream, lotion, powder, shampoo and lipstick, were extracted under uhrasonication. The extract was centrifuged, and the upper solution was concentrated by rotary evaporator. The recon-structed solution was then cleaned up by Sep-Pak Silica solid phase extraction cartridge. Qualitative and quan- titative analysis was carried out under the MRM mode after the chromatographic separation on DB-5 MS （30m×0.25mm,0.25μm） capillary column. The limit of quantitation （LOQ） for musk xylene was 5 μg/kg. The mean recoveries at the three spiked levels of 5-50μg/kg were 81.1%-86.9% , with the intra-day precision less than 10% and the inter-day precision less than 12%. The method is accurate, rapid, sensitive and adapt to the inspection of musk xylene in cosmetics.