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[毛细管气相色谱法分析化妆品中的邻苯二甲酸酯]

[Analysis of the phthalates in cosmetics by capillary gas chromatography].

作者信息

Chen Huiming, Wang Chao, Wang Xing

机构信息

China Import & Export Commodity Inspection Technology Institute, Beijing 100025, China.

出版信息

Se Pu. 2004 May;22(3):224-7.

Abstract

A capillary gas chromatographic method with flame ionization detector (GC-FID) for the detection of the six phthalates (dimethyl phthalate (DMP), diethyl phthalate (DEP), di-n-butyl phthalate (DBP), butyl benzyl phthalate (BBP), di(2-ethylhexyl) phthalate (DEHP), di-n-octyl phthalate (DOP)) in the cosmetics was developed. The phthalates were extracted from cosmetics with methanol under ultrasonication and then separated with high-speed centrifugation. The supernatant was dehydrated and filtrated through membrane with 0.5 microm pore diameter. The filtrate was injected into the GC system for analysis. Then the positive results observed in the GC-FID chromatogram were confirmed by gas chromatography-electron impact-mass detection (GC-EI-MS) analysis. Retention times of the peaks could be applied for qualitative analysis. External standard method was used for quantitative analysis. The recoveries of the six phthalates were between 82.90% and 109.50%. The relative standard deviations were between 2.1% and 4.6%. The detection limits of the method were: 0.1 ng for DMP, DEP, DBP and BBP, and 0.5 ng for DEHP and DOP, respectively. The method presented the advantages of high precision, high sensitivity, small sample size, and simple pretreatment. The method can be used to test the six phthalates in the cosmetics.

摘要

建立了一种采用火焰离子化检测器(GC-FID)的毛细管气相色谱法,用于检测化妆品中的六种邻苯二甲酸酯(邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二正丁酯(DBP)、邻苯二甲酸丁苄酯(BBP)、邻苯二甲酸二(2-乙基己基)酯(DEHP)、邻苯二甲酸二正辛酯(DOP))。用甲醇在超声条件下从化妆品中提取邻苯二甲酸酯,然后通过高速离心进行分离。将上清液脱水并通过孔径为0.5微米的膜过滤。将滤液注入气相色谱系统进行分析。然后通过气相色谱-电子轰击-质谱检测(GC-EI-MS)分析确认在GC-FID色谱图中观察到的阳性结果。峰的保留时间可用于定性分析。采用外标法进行定量分析。六种邻苯二甲酸酯的回收率在82.90%至109.50%之间。相对标准偏差在2.1%至4.6%之间。该方法的检测限分别为:DMP、DEP、DBP和BBP为0.1纳克,DEHP和DOP为0.5纳克。该方法具有精密度高、灵敏度高、进样量小和预处理简单等优点。该方法可用于检测化妆品中的六种邻苯二甲酸酯。

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