第 27 卷第 6 期 高 校 化 学 工 程 学 报 No.6
Vo l . 2 7
2013 年 12 月 Journal of Chemical Engineering of Chinese Universities Dec.
2013
文章编号:1003-9015(2013)06-0974-06
分散液液微萃取-气相色谱联用检测果汁中有机磷类农药残留
张雪莲
1
, 张耀海
2
, 焦必宁
1,2
, 苏学素
3
, 艾春平
3
(1. 西南大学 食品科学学院, 重庆 400715; 2. 农业部 柑橘产品质量安全风险评估实验室,
西南大学柑橘研究所, 重庆 400712; 3. 西南大学 化学化工学院, 重庆 400716)
摘 要:如何检测果汁中的痕量农药残留是一个重要问题。今研究建立了分散液液微萃取(DLLME)结合气相色谱-火焰
光度检测 (GC-FPD)法检测果汁中 8 种有机磷农药残留新方法,并对影响液液微萃取效果的因素(如萃取剂和分散剂类
型及用量、萃取时间和盐浓度等)进行了优化。在优化条件下,8 种有机磷的富集倍数可达 106~147;检出限 ( S /N = 3)
介于 0.034~0.153 μgL
1
。建立的新方法可用于多种果汁中农药多种残留检测,其平均加标回收率在 74.7%~128.0%,
相对标准偏差小于 5.6%,完全满足果汁中有机磷类农药多种残留的检测要求。
关键词:分散液液微萃取;有机磷类农药;气相色谱;果汁
中图分类号:TQ450.263 文献标识码:A DOI:10.3969/j.issn.1003-9015.2013.06.009
Determination of Organophosphorous Pesticide Residues in Fruit Juices Samples Using
Dispersive Liquid-liquid Microextraction Coupled with Gas Chromatography
ZHANG Xue-lian
1
, ZHANG Yao-hai
2
, JIAO Bi-ning
1,2
, SU Xue-su
3
, AI Chun-ping
3
(1. College of Food Science, Southwest University, Chongqing, 400715, China; 2. Laboratory of Quality &
Safety Risk Assessment for Citrus Products of Ministry of Agriculture, Citrus Research Institute, Southwest
University, Chongqing 400712, China; 3. College of Chemistry and Chemical Engineering, Southwest
University, Chongqing 400716, China)
Abstract: How to determine trace multipesticide residues in fruit juices is an important problem. In this paper,
a novel method was developed for the analysis of eight organophosphorus pesticide residues in fruit juice by
using dispersive liquid-liquid microextraction(DLLME) coupled with gas chromatography-flame photometric
detector (GC-FPD). Parameters affecting the extraction performance, such as the species and volume of
extraction and dispersive solvents, extraction time and salt concentration, were studied and optimized. Under
the optimum extraction conditions, the enrichment factors range from 106 to 147 for eight kinds of
organophosphorus pesticides, and the detection limits of the method are in the range of 0.034~0.153 μgL
1
. The
developed method was successfully applied for the determination of multipesticide residues in various fruit
juices, and the average spiked recoveries range from 74.7% to 128.0%, and relative standard deviations is less
than 5.6%. Results show that the method proposed could completely meet the requirement for the determination
of pesticide residues in fruit juices.
Key words: dispersive liquid-liquid microextraction (DLLME); organophosphorus pesticides;
gas chromatography(GC); fruit juices
1 前 言
随着人们生活水平的提高和健康知识的普及,越来越多的消费者开始选择有利于健康的果汁饮品。
收稿日期:2012-04-02;修订日期:2012-10-29。
基金项目:“十一五”国家科技支撑计划项目(2009BADB7B04);公益性行业(农业)科研专项(200903054);现代农业(柑橘)产业技术体系建设专项(CARS-27);重
庆市自然科学基金重点项目(cstc2013jjB80009)。
作者简介:张雪莲(1987-),女,山东菏泽人,西南大学硕士生。通讯联系人:焦必宁,E-mail:bljiao@tom.com