同位素稀释-气相色谱-串联质谱法测定化妆品中10种合成麝香  

Determination of 10 Synthetic Musks in Cosmetics by Isotope Dilution-GC-MS/MS

作　　者：周静[1] 张晓岚[2] 徐红斌[1] ZHOU Jing;ZHANG Xiao-lan;XU Hong-bin(Shanghai Institute of Quality Inspection and Technical Research,Shanghai 200233,China;Institute of Environmental Pollution and Health,School of Environmental and Chemical Engineering,Shanghai University,Shanghai 200444,China)

机构地区：[1]上海市质量监督检验技术研究院,上海200233 [2]上海大学环境与化学工程学院,环境污染与健康研究所,上海200444

出　　处：《质谱学报》2018年第4期482-490,共9页Journal of Chinese Mass Spectrometry Society

摘　　要：建立了同位素稀释-气相色谱-串联质谱(GC-MS/MS)法同时测定化妆品中10种合成麝香(SMs),并对方法前处理和仪器条件进行了优化。样品加入氘代同位素内标后,以饱和氯化钠-正己烷溶液体系超声提取,提取液经氮吹浓缩定容后,采用极性毛细管柱VF-WAXms(30 m×0.25 mm×0.25μm)分离,以多反应监测模式(MRM)测定,内标校正标准曲线法定量。结果表明:10种合成麝香的线性范围为1.0~100.0μg/L,相关系数均大于0.99,定量限为1.0~8.0μg/kg。加标回收率在92.5%~102.0%之间,相对标准偏差(RSD)均小于5%。本方法简便、准确、快速、灵敏,可同时检测化妆品中10种合成麝香成分。As the cheap substitutes of natural musks, large quantities of synthetic musks （SMs） were manufactured and added in a wide variety of cosmetics for the distinct flavor as well as their abilities to improve the fixation of compounds and to round off fragrance compositions. However, with the in-depth research on synthetic musks, these compounds have been described as a new group of bioaccumulative and persistent xenobiotics. Much attention has been given to the level of synthetic musks in daily cosmetic products. In this study, a comprehensive analytical method based on isotope dilution-gas chromatography-triple quadrupole mass spectrometry （GC-MS/MS） was developed and optimised for simultaneous determination of ten kinds of SMs in cosmetics. Cosmetic samples were spiked with deuterium-labeled isotope internal standards （ d 3-AHTN and d 15 -MX）. Then 1.0 mL saturated sodium chloride and 2.0 mL n -hexane were added to the above sample to extract the target compounds. Ultrasonic extraction （20 min at 40 ℃ ） was chosen as the sample pretreatment method according to the results of the optimization experiments. The solution was centrifugated at 8 000 r/min for 3 min. The upper layer extraction solution was transfered and the remaining sample solution was cleaned twice with 2.0 mL n -hexane, respectively. After combining all the supernatant, the collected solution was evaporated with nitrogen and determined by GC-MS/MS. The conditions of GC-MS/MS were developed for simultaneous determination of ten SMs in cosmetic samples under the MRM mode. All compounds were separated by VF-WAXms capillary column, with which all targets could be detected with a clear baseline separation. Quantitative analysis was carried out using internal standard correction standard curve calibration. The results showed that ten SMs could reach a good linear relationship with the concentration range of 1.0-100.0 μg/L and the correlation coefficients were all more than 0.99. The limits of quantitation （LOQs） of SMs were 1.0-8.0

关 键 词：合成麝香 同位素稀释 气相色谱-串联质谱(GC-MS/MS)化妆品 

分 类 号：O657.63[理学—分析化学]