超声辅助分散液液微萃取-高效液相色谱测定护肤水中9种荧光增白剂  

Simultaneous Determination of Nine Fluorescent Whitening Agents in Skincare Water Using Ultrasound-assisted Dispersive Liquid-Liquid Microextraction Coupled with High Performance Liquid Chromatography

作　　者：张宪臣 华洪波 薄艳娜 李蓉 张朋杰 杨芳 王勇 熊仁广 

机构地区：[1]中山出入境检验检疫局检验检疫技术中心,广东中山528403 [2]中山市卓雅外国语学校,广东中山528401 [3]暨南大学包装工程研究所,广东普通高校产品包装与物流重点实验室,广东珠海519070

出　　处：《分析测试学报》2016年第11期1451-1455,共5页Journal of Instrumental Analysis

基　　金：国家质检总局科技计划项目(2015IK052);中山市科技计划项目(2014A2FC241);广东检验检疫局科技计划项目(2015GDK32)

摘　　要：建立了超声辅助分散液液微萃取技术结合高效液相色谱配荧光检测器（UA-DLLME-HPLC-FLD）同时测定护肤水中9种荧光增白剂（FWAs）残留量的检测方法。考察了萃取剂的种类与体积、分散剂的种类与体积分数、盐效应、pH值、超声时间等因素对萃取效果的影响,确定最佳萃取条件：50μL三氯甲烷为萃取剂,250μL甲醇为分散剂,氯化钠用量为0.20 g,4 500 r/min离心2 min。在优化条件下,9种荧光增白剂在一定质量浓度范围内线性关系良好,相关系数均大于0.999 0,方法检出限（S/N=3）为0.06~4.20 mg/kg,定量下限（S/N≥10）为0.2~14.0 mg/kg,方法的平均回收率为84.3%~102.4%。该方法具有有机溶剂用量少、操作简单、快捷、灵敏等优点。A method based on ultrasonic-assisted dispersive emulsion microextraction procedure coupled to high performance liquid chromatography with fluorescence detector （ UA - DLLME - HPLC - FLD） was developed for the determination of nine fluorescent whitening agents （FWAs） residues in skincare water. Experimental conditions affecting the microextraction procedure such as type and volume of extraction solvent, content of disperse solvent, salt concentration, pH value, extraction time and centrifugal time were investigated. The ultrasonic-assisted disperse emulsion microextraction con- ditions were optimized by using 50 μL chloroform as solvent and 250 μL methanol as disperser sol- vent, and the mixture was centrifuged at 4 500 r/min for 2 min. Under the optimum conditions, the calibration curves of nine fluorescent whitening agents in a certain concentration range with correlation coefficients more than 0. 999 0. The limits of detection （LODs） of night fluorescent whitening agents ranged from 0.06 mg/kg to 4. 20 mg/kg and the limits of quantitation（LOQs） ranged from 0. 2 mg/kg to 14. 0 mg/kg. The average recoveries for nine fluorescent whitening agents residues in skincare wa-ter were in the range of 84. 3% - 102.4%. Compared to the previous methods, the new procedure has the characteristics of simple sample preparation, low organic solvent consumption and high sensitivity.

关 键 词：分散液液微萃取 超声辅助 高效液相色谱 荧光增白剂(FWAs) 护肤水 

分 类 号：O657.72[理学—分析化学] TQ610.495[理学—化学]