气相色谱-质谱法测定化妆品中17种防腐剂的含量  

Determination of the Contents of Seventeen Kinds of Preservative in Cosmetic by GC-MS

作　　者：许勇[1] 钟吉强[1] 郑荣[1] XU Yong;ZHONG Jiqiang;ZHENG Rong(Shanghai Institute of Food and Drug Control/NMPA Key Laboratory for Monitoring and Evaluation of Cosmetics,Shanghai 201203,China)

机构地区：[1]上海市食品药品检验所/国家药品监督管理局化妆品监测评价重点实验室,上海201203

出　　处：《香料香精化妆品》2020年第6期72-79,共8页Flavour Fragrance Cosmetics

摘　　要：为建立以气相色谱-质谱法测定化妆品中17种防腐剂含量的方法,根据化妆品的不同基质分别采用甲醇直接提取和沉淀试剂沉淀的方法对样品进行净化处理。采用质量分数6%氰丙基苯基-94%二甲基聚硅氧烷为固定相的DB-624毛细管色谱柱(30 m×250μm×1.4μm)进行气相分离,然后测定。结果发现:三氯叔丁醇等16种化合物线性范围为0.2~10μg/mL;甲基氯异噻唑啉酮线性范围为0.02~1μg/mL。它们的相关系数r值均大于0.999。三氯叔丁醇等16种化合物检出质量比为15 mg/kg;甲基氯异噻唑啉酮检出质量比为1.5 mg/kg。平均加样回收率(n=9)范围为86.2%~111.8%。所建立方法灵敏度高、专属性好、操作简便、重现性优。A method was developed for simultaneously determining the content of 17 kinds of preservative in cosmetic products by GC-MS.According to the different substrates of cosmetics,the samples were extracted by methanol or precipitated by precipitation reagent,then analyzed by GC-MS on the DB-624 column(30 m×250μm×1.4μm)with mass fraction of 6%cyanopropylphenyl-94%dimethyl polysiloxane as stationary phase.Test results showed that calibration curves of 16 compounds including chlorobutanol and others were linear in the ranges of 0.2 to 10μg/mL,that of 5-chloro-2-methylisothiazolone was linear in the range of 0.02 to 1μg/mL.The detection limit of 5-chloro-2-methylisothiazolone was 1.5 mg/kg.The detection limits of 16 compounds including chlorobutanol and others were 15 mg/kg.The average recoveries were 86.2%to 111.8%(n=9).The method established is simple,sensitive,accurate,specific and reproducible.

关 键 词：气相色谱-质谱法 防腐剂 化妆品 甲基氯异噻唑啉酮 三氯叔丁醇 

分 类 号：O657.63[理学—分析化学] TQ658[理学—化学]