摘要
目的:建立同时测定化妆品中7个含卤素类防腐剂(三氯叔丁醇、5-溴-5-硝基-1,3-二噁烷、三氯卡班、二氯苯甲醇、碘丙炔醇丁基氨甲酸酯、三氯生、氯咪巴唑)的气相色谱-电子捕获检测器(GC-ECD)分析方法。方法:样品用甲醇超声提取,经无水硫酸钠脱水,样品溶液经DB-5MS(30 m×0.25 mm×0.25μm)毛细管色谱柱分离,电子捕获检测器(ECD)检测,外标法定量。结果:7个含卤素类防腐剂质量浓度在0.04~10.0μg·mL^(-1)范围内线性关系良好,相关系数均不小于0.99;方法检测下限(S/N=3)为0.32~4μg·g^(-1);在液态水基类、凝胶类、乳液类样品中进行加标试验,平均回收率为84.4%~98.8%,RSD(n=6)为2.3%~6.3%从本市抽检的54批样品中检出碘丙炔醇丁基氨甲酸酯4份,检出三氯生1份。结论:本方法准确可靠,适用于化妆品中7个含卤素类防腐剂的同时检测。
Objective：To establish an analytical method for simultaneous detection of 7 kinds of halogenated preservatives in cosmetic products（chlorobutanol,5-bromo-5-nitro-1,3-dioxane,triclocarban,2,4-dichlorobenzyl alcohol,iodopropynyl butylcarbamate,triclosan,and climbazole）with gas chromatography-electron capture detector.Methods：After ultrasonic extraction in methanol,dried over anhydrous sodium sulfate,the extractive liquid was injected and separated on DB-5 MS capillary column（30 m×0.25 mm×0.25 μm）.The target components were detected using electron capture detector（ECD）and quantified by external standard method.Results：7 kinds of halogenated preservatives had good linearity（r ≥ 0.99）in the concentration of 0.04-10.0 μg·mL^（-1）.The detection limits of target compounds with this method（LODs,S/N=3）ranged from 0.32 μg·g^（-1） to 4 μg·g^（-1）.Spike recovery experiments were performed on 7 kinds of halogenated preservatives in water-based cosmetics,gel,emulsion samples.Therecovery rates were in the range of 84.4%-98.8%,with RSD（n=6）of 2.3%-6.3%.From the 54 batches of samples, 4 copies of iodopropynyl butylcarbamate were detected, and 1 triclosan samples was detected.Conclusion：This accurate and precise method could be applied to the simultaneous detection of 7 kinds ofhalogenated preservatives in cosmetic products.
作者
钟吉强
郑荣
陈丹丹
刘畅
王柯
ZHONG Ji-qiang;ZHENG Rong;CHEN Dan-dan;LIU Chang;WANG Ke(Shanghai Institute for Food and Drug Control, Shanghai 201203, China)
出处
《药物分析杂志》
CAS
CSCD
北大核心
2018年第5期806-811,共6页
Chinese Journal of Pharmaceutical Analysis
