摘要
该文基于QuEChERS法结合气相色谱-串联质谱法(GC-MS/MS),建立了测定膏霜类化妆品中非法添加本维莫德的方法。样品经饱和氯化钠溶液分散后乙腈提取,无水硫酸镁、PSA和C18组成的净化剂净化后,以Agilent VF-17ms毛细管柱(30 m×0.25 mm×0.25μm)分离,在选择反应监测(SRM)模式下检测,以基质匹配外标法定量。通过考察提取溶剂种类、提取溶剂体积、提取时间、净化剂组成及用量对本维莫德回收率的影响,确定最优前处理方法。在优化条件下,本维莫德在1~100μg/L范围内呈良好线性关系,相关系数(r^(2))为0.9995;方法检出限为0.005μg/g,方法定量下限为0.02μg/g,目标物的加标回收率为90.0%~96.3%,重复性相对标准偏差(RSD,n=6)为1.5%~2.7%,日内和日间精密度(RSD)均小于10%。采用该方法对采集的90个膏霜样品进行检测,检出1个阳性样品。该方法具有简便、快速、准确及灵敏的优点,可为打击化妆品非法添加和保障化妆品的质量安全提供技术支撑。
A method of QuEChERS/gas chromatography-tandem mass spectrometry(GC-MS/MS)was established for the determination of benvitimod added illegally in cream cosmetics.Cream sam⁃ples were dispersed with saturated sodium chloride solution and extracted with acetonitrile.After pu⁃rified with anhydrous magnesium sulfate,PSA and C18,the pretreatment samples were separated on an Agilent VF-17ms capillary column(30 m×0.25 mm×0.25μm),detected by GC-MS/MS in selective reaction monitoring(SRM)mode,and quantified by the matrix-matched calibration.The pretreatment method was optimized by investigating the effects of type and volume of extraction sol⁃vent,extraction time,purification composition and dosage on the recovery of benvitimod.Under the optimal conditions,benvitimod showed a good linear relationship in the concentration range of 1-100μg/L with a correlation coefficient(r^(2))of 0.9995.The limit of detection was 0.005μg/g,and the limit of quantitation was 0.02μg/g.The spiked recoveries for the target substance ranged from 90.0%to 96.3%,with relative standard deviations(RSDs,n=6)for repeatability of 1.5%-2.7%,and inter-RSDs and intra-RSDs both less than 10%.The method was applied to the determi⁃nation of 90 cream cosmetics containing plant extracts,in which one positive sample was found.This method is convenient,accurate and sensitive,and it could provide a technical support for com⁃bating illegal addition of cosmetics and ensuring the quality and safety of cosmetics.
作者
梁梓洋
罗辉泰
周熙
林晓珊
吴惠勤
黄芳
LIANG Zi-yang;LUO Hui-tai;ZHOU Xi;LIN Xiao-shan;WU Hui-qin;HUANG Fang(Institute of Analysis,Guangdong Academy of Sciences(China National Analytical Center,Guangzhou),Guangdong Provincial Key Laboratory of Chemical Measurement and Emergency Test Technology,Guangdong Provincial Engineering Research Center for Quality and Safety of Traditional Chinese Medicine,Guangzhou 510070,China)
出处
《分析测试学报》
CAS
CSCD
北大核心
2023年第6期762-767,共6页
Journal of Instrumental Analysis
基金
国家药品监督管理局化妆品风险评估重点实验室开放课题(KF2022007)。
