摘要
建立了用毛细管气相色谱配氢火焰离子化检测器测定化妆品中6种酞酸酯(邻苯二甲酸二甲酯(DMP)、邻苯二甲酸二乙酯(DEP)、邻苯二甲酸二丁酯(DBP)、邻苯二甲酸丁基苄基酯(BBP)、邻苯二甲酸二(2 乙基己)酯(DEHP)和邻苯二甲酸二正辛酯(DOP))的方法。样品用甲醇超声提取,经高速冷冻离心,清液经干燥脱水过0 5μm滤膜过滤,直接注入气相色谱仪进行分析。然后,经过气相色谱 电子电离 质谱检测分析,确证气相色谱 氢火焰检测的阳性检出结果。用保留时间定性,外标法定量。6种酞酸酯的回收率为82 90%～109 50%;精密度(以相对标准偏差表示)为2 1%～4 6%;DMP、DEP、BBP和DBP的检测限(以信噪比为3计)均为0 1ng,DEHP和DOP为0 5ng。该方法准确度和灵敏度高,样品用量少,前处理简单,可同时测定化妆品中6种酞酸酯化合物。
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 supernatent was dehydrated and filtrated through membrane with 0.5 μm 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.
出处
《色谱》
CAS
CSCD
北大核心
2004年第3期224-227,共4页
Chinese Journal of Chromatography
关键词
毛细管气相色谱
酞酸酯
化妆品
capillary gas chromatography
phthalates
cosmetics
