PDF《气相色谱 - 电子捕获检测器法同时检测化妆品中 7 个防腐剂》

・806・ 气相色谱 - 电子捕获检测器法同时检测化妆品中

7 个防腐剂 钟吉强, 郑荣, 陈丹丹, 刘畅, 王柯 * (上海市食品药品检验所, 上海 201203) 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f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 μ m) 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0.04~10.0μ g・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0.32~4μ g・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. 关键词: 气相色谱 - 电子捕获检测器法;

化妆品检测;

含卤素类防腐剂;

三氯叔丁醇;

5- 溴-5- 硝基 -1, 3- 二f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 中图分类号: R

917 文献标识码: A 文章编号: 0254-1793 (2018) 05-0806-06 doi: 10.16155/j.0254-1793.2018.05.11 Detection of

7 kinds of preservatives in cosmetics by gas chromatography with electron capture detector ZHONG Ji-qiang, ZHENG Rong, CHEN Dan-dan, LIU Chang, WANG Ke* (Shanghai Institute for Food and Drug Control, Shanghai 201203, China) Abstract 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 μ g・mL-1 . The detection limits of target compounds with this method (LODs, S/N=3) ranged from 0.32 μ g・g-1 to

4 μ g・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 * 通信作者 Tel: (021) 50798196;

E-mail: [email protected] 第一作者 Tel: (021) 20428210;

E-mail: [email protected] ・807・ 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. Keywords;

gas chromatography-electron capture detector;

cosmetics detection;

halogenated preservative;

chlorobutanol;

5-bromo-5-nitro-1, 3-dioxane;

triclocarban;

2, 4-dichlorobenzyl alcohol;

iodopropynyl butylcarbamate;