吹扫捕集-气相色谱-串联质谱法测定化妆品中1,4-二恶烷  

Determination of 1,4-dioxane in cosmetics by purge and trap coupled with gas chromatography-tandem mass spectrometry

作　　者：程焰芳[1] 甘平胜[1] 潘心红[1] 柳华春[1] 谢进[1] CHENG Yan- fang, GAN Ping- sheng, PAN Xin- hong, LIU Hua- chun, XIE Jin(Guangzhou Center for Disease Control and Prevention, Guangzhou , Guangdong 510440, Chin)

机构地区：[1]广州市疾病预防控制中心,广东广州510440

出　　处：《中国卫生检验杂志》2018年第5期528-530,共3页Chinese Journal of Health Laboratory Technology

基　　金：广州市医药卫生科技项目(20171A011278)

摘　　要：目的建立化妆品中二恶烷的吹扫捕集-GC-MS/MS测定方法。方法利用吹扫捕集-GC-MS/MS联用仪,采用多级反应监测(MRM)扫描模式,选择m/z 88为母离子、定性子离子m/z 58和定量子离子m/z 57测定化妆品中二恶烷的含量。结果通过优化吹扫条件,减少解吸时间为0.25 min,得到的1,4-二恶烷的峰形最完美;减少吹扫时间为6 min,1,4-二恶烷吹扫效率最高。在所建立的实验条件下,二恶烷的线性范围为0μg/ml^100μg/ml,回归方程为y=2 327x-7 016,相关系数为0.999 5,方法的检出限为0.015μg/g。样品的加标回收率为92.4%~98.9%,相对标准差(RSD)为1.52%~3.06%。结论本方法采用的MRM扫描模式有效消除了复杂基质的干扰,所建立的分析方法操作简便、准确、灵敏、快速,可用于化妆品中痕量二恶烷的测定。Objective To establish a method for the determination of 1,4-dioxane in cosmetics by purge and trap coupled with gas chromatography-tandem mass spectrometry（ GC-MS/MS）. Methods 1,4-dioxane in cosmetics was determined by purge and trap coupled with GC-MS/MS in multiple reaction monitoring（ MRM） scanning mode. m/z 88 was selected as parent ion,m/z 58 was selected as qualitative daughter ion and m/z 57 was selected as quantitative daughter ions. Results By optimizing the purge conditions,the desorption time was reduced to 0. 25 min,and the peak of 1,4-dioxane was perfect;when the purge time was reduced to 6 min,the pruge efficiency of 1,4-dioxane reached to the highest. Under the optimal experimental conditions,the determination limited of dioxane was within 0 μg/ml-100 μg/ml. The regression equation was y = 2 327 x-7 016,the correlation coefficient（ r） was 0. 999 5,and the detection limit of the method was 0. 015 μg/g. The spiked recoveries of the samples were within 92. 4%-98. 9%,and the relative standard deviation（ RSD） was within 1. 52%-3. 06%. Conclu sion The MRM scanning mode adopted in this method can effectively eliminate the interference of complex matrix. The established method is simple,accurate,sensitive and rapid,and can be used for the determination of trace dioxane in cosmetics.

关 键 词：吹扫捕集 气相色谱-串联质谱 二恶烷 

分 类 号：O657.63[理学—分析化学]