气相色谱-串联质谱法测定化妆品中7种二甲基环硅氧烷  

Determination of Seven Dimethylcyclosiloxanes in Cosmetics by Gas Chromatography-Tandem Mass Spectrometry

作　　者：李思源[1] 陈安丽[1] 赵思雯 严小红[1] 丁怡[1] LI Si-yuan;CHEN An-li;ZHAO Si-wen;YAN Xiao-hong;DING Yi(Guangzhou Institute for Drug Control,Guangzhou 510160,China)

机构地区：[1]广州市药品检验所,广东广州510160

出　　处：《分析测试学报》2023年第12期1607-1614,共8页Journal of Instrumental Analysis

摘　　要：建立了气相色谱-串联质谱法(GC-MS/MS)测定化妆品中7种二甲基环硅氧烷的检测方法。将不同基质化妆品经异丙醇分散、正己烷提取后,以HP-5MS UI毛细管色谱柱(30 m×0.25 mm×0.25μm)分离,采用GC-MS/MS多重反应监测(MRM)模式检测,基质匹配外标法定量。结果显示,7种二甲基环硅氧烷在50~1000 ng/mL范围内线性关系良好,相关系数(R)为0.9965~0.9999;方法检出限(LOD)为4.0~6.1 mg/kg,定量下限(LOQ)为13.2~20.4 mg/kg,平均加标回收率为85.1%~115%,相对标准偏差(RSD)为0.90%~7.0%。采用该方法对市售的102批化妆品进行检测,检出组分涵盖了D4~D9。该方法简便、快速、灵敏、准确,适用于化妆品中7种二甲基环硅氧烷的监测,为保障化妆品的质量安全提供了技术支撑。A gas chromatography-tandem mass spectrometric(GC-MS/MS)method was developed for the simultaneous determination of 7 dimethylcyclosiloxanes in cosmetics.Cosmetics samples with different matrices were dispersed with isopropyl alcohol and extracted with n-hexane,then separated on a HP-5MS UI capillary column(30 m×0.25 mm×0.25μm),and detected by GC-MS/MS in mul⁃tiple reactive ion monitoring(MRM)mode.The data were processed and quantified using the matrixmatched external standard method.The results showed that the 7 dimethylcyclosiloxanes had good linear relationships in the range of 50-1000 ng/mL,with correlation coefficients(R)of 0.9965-0.9999.The limits of detection(LODs)and the limits of quantitation(LOQs)were in the range of 4.0-6.1 mg/kg and 13.2-20.4 mg/kg,respectively.The average recoveries were in the range of 85.1%-115%,with relative standard deviations(RSDs)of 0.90%-7.0%.The method was applied to test 102 batches of cosmetics sold on the market,and the detected components covered D4-D9.The method is convenient,fast,sensitive and accurate,which is suitable for the determination of the 7 dimethylcyclosiloxanes in cosmetics and could provide technical support for ensuring the quality and safety of cosmetics.

关 键 词：气相色谱-串联质谱(GC-MS/MS) 二甲基环硅氧烷 化妆品 

分 类 号：O657.71[理学—分析化学] O141.4[理学—化学]