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×0.25 μm）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-5MS 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.The recovery 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 of halogenated preservatives in cosmetic products.
