气相色谱-串联质谱法结合QuEChERS方法快速检测柑橘中52种农药多残留

doi:10.7506/spkx1002-6630-201306033

食品科学 ›› 2013, Vol. 34 ›› Issue (6): 152-155.doi: 10.7506/spkx1002-6630-201306033

气相色谱-串联质谱法结合QuEChERS方法快速检测柑橘中52种农药多残留

张雪莲1，张耀海2，焦必宁1,2,3,*

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(重庆)，中国农业科学院柑桔研究所，重庆 400712；3.国家柑桔工程技术研究中心，重庆 400712

收稿日期:2012-03-16 修回日期:2013-01-28 出版日期:2013-03-25 发布日期:2013-03-01
通讯作者: 张雪莲 E-mail:zhangxuelianjob@126.com

Rapid Determination of 52 Pesticide Residues in Citrus by Gas Chromatography-Tandem Mass Spectrometry Coupled with QuEChER

ZHANG Xue-lian1，ZHANG Yao-hai2，JIAO Bi-ning1,2,3,*

1. College of Food Science, Southwest University, Chongqing 400715, China；2. Laboratory of Quality & Safety Risk Assessmentfor Citrus Products (Chongqing), Ministry of Agriculture, Citrus Research Institute, Chinese Academy of Agricultural Sciences,Chongqing 400712, China；3. National Citrus Engineering Research Center, Chongqing 400712, China

Received:2012-03-16 Revised:2013-01-28 Online:2013-03-25 Published:2013-03-01

摘要/Abstract

摘要： 建立气相色谱-串联质谱结合QuEChERS方法快速检测柑橘中52种农药多残留。样品经乙腈提取、无水硫酸镁和氯化钠盐析后，用N-丙基乙二胺(PSA)固相材料分散填料净化，用气相色谱-串联质谱在多反应监测模式(MRM)下分析检测，该方法的检出限(RSN=3)为0.07～5.7μg/kg，平均回收率为77.3%～117.8%，相对标准偏差小于13.8%。该方法简单、快速、安全、便宜、重现性好，适用于柑橘类水果农药多残留检测。

关键词: 柑橘, 农药残留, QuEChERS, 气相色谱-串联质谱法

Abstract: In this study, an analytical method was established for the determination of 52 pesticide residues in citrus fruits using QuEChERS cleanup and gas chromatography-tandem mass spectrometry (GC-MS/MS). The pesticide residues in citrus fruit samples were extracted into acetonitrile and salted out by anhydrous MgSO4 and NaCl. Then, the pesticide residues in the supernatant after clean-up on the sorbents of N-propyl ethylene diamine (PSA) were subjected to GC-MS/MS analysis under multi-reaction monitoring (MRM) mode. The limit of detection (RSN = 3) of the established method were in the range of 0.07–5.7 μg/kg, and the average recovery rates for 52 pesticide residues in a blank sample were 77.3%–117.8% with a relative standard deviation (RSD) less than 13.8%. Therefore, this method is simple, quick, safe, cheap and reproducible so that it is suitable for the detection of multiple pesticide residues in citrus fruit samples.

Key words: citrus, pesticide residue, QuEChERS, gas chromatography-tandem mass spectrometry (GC-MS/MS)

中图分类号:

S481.8

张雪莲1，张耀海2，焦必宁1,2,3,*. 气相色谱-串联质谱法结合QuEChERS方法快速检测柑橘中52种农药多残留[J]. 食品科学, 2013, 34(6): 152-155.

ZHANG Xue-lian1，ZHANG Yao-hai2，JIAO Bi-ning1,2,3,*. Rapid Determination of 52 Pesticide Residues in Citrus by Gas Chromatography-Tandem Mass Spectrometry Coupled with QuEChER[J]. FOOD SCIENCE, 2013, 34(6): 152-155.

参考文献

Cunha S C, Lehotay S J, Mastovska K, et al. Evaluation of the QuEChERS sample preparation approach for the analysis of pesticide residues in olives[J].Journal of Separation Science, 2007,30(4): 620-632.
Paya P, Anastassiades M, Mack D, et al. Analysis of pesticide residues using the Quick Easy Cheap Effective Rugged and Safe (QuEChERS) pesticide multiresidue method in combination with gas and liquid chromatography and tandem mass spectrometric detection[J]. Analytical and Bioanalytical Chemistry, 2007, 389(6): 1697-1714.
宋莹, 张耀海, 黄霞, 等. 气相色谱-串联质谱法快速检测水果中的多效唑残留[J]. 分析化学, 2011, 39(8): 1270-1273.
Angelika W, Marek B. Determination of pesticide residues in food matrices using the QuEChERS methodology[J]. Food Chemistry, 2011, 125(3): 803-812.
Lehotay S J, Son K A, Kwon H. Comparison of QuEChERS sample preparation methods for the analysis of pesticide residues in fruits and vegetables[J]. Journal of Chromatography A, 2010, 1217(16): 2548-2560.
Lehotay S J, De K A, Hiemstra M, et al. Validation of a Fast and Easy Method for the Determination of Residues from 229 Pesticides in Fruits and Vegetables Using Gas and Liquid Chromatography andMass Spectrometric Detection[J]. Journal of AOAC International, 2005, 88(2): 595-614.
Nguyen T D, Yu J E, Lee D M, Lee G H. A multiresidue method for the determination of 107 pesticides in cabbage and radish using QuEChERS sample preparation method and gas chromatography mass spectrometry[J]. Food Chem., 2008, 110 (1): 207-213.
Anastassiades M, Lehotay S J, Stajnbaher D, Schenck F J. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticideresidues in produce[J]. J AOAC International, 2003, 86(2): 21, 421-431.
Lesueur C, Knittl P, Gartner M, et al. Analysis of 140 pesticides from conventional farming foodstuff samples after extraction with the modified QuECheRS method[J]. Food Control, 2008, 19(9): 906-914.
Nguyen T D, Fu J E, Lee D M, et al. A multiresidue method for the determination of 107 pesticides in cabbage and radish using QuEChERS sample preparation methodand gas chromatography mass spectrometry[J]. Food Chemistry, 2008, 110(1): 207-213.
Wilkowska A, Biziuk M. Determination of pesticide residues in food matrices using the QuEChERS Methodology[J]. Food Chemistry, 2011,125(3): 803-812.
苏建峰, 胡朝阳, 陈劲星, 等. 气相色谱-质谱联用快速检测毛豆中103种农药多残留 [J]. 分析试验室，2009, 28(6): 84-89.
沈伟健, 余可垚, 桂茜雯, 等. 分散固相萃取-气相色谱-串联质谱法测定蔬菜中107种农药的残留量[J]. 色谱, 2009, 27(4): 391-400.
宋淑玲, 李重九, 马晓东, 等. 蔬菜中残留农药的石墨化碳黑净化和气相色谱-质谱检测方法[J]. 分析化学, 2008, 36(11): 1526-1530.
张耀海, 赵其阳, 焦必宁, 等. 气相色谱-质谱联用快速检测柑橘中55种农药多残留[J]. 食品与发酵工业, 2010, 36(7): 135-138.

[1]	连玉晶，周一冉，孙欣，陈佳楠，郑振佳，王明林. 基于胺基功能化磁性纳米粒子改进QuEChERS方法结合GC-MS/MS检测果蔬中7 种农药残留[J]. 食品科学, 2021, 42(4): 297-304.
[2]	朱晓玲，刘杰，余婷婷，张莉，王会霞，吴婉琴，曹琦，张亚珍，杨总. 高效液相色谱-四极杆-飞行时间质谱法快速筛查胡椒粉中多种农药残留[J]. 食品科学, 2021, 42(4): 287-296.
[3]	范传会，何建军，陈学玲，王少华. 乳酸钙对高酯柑橘果胶乳化性的影响[J]. 食品科学, 2021, 42(4): 44-50.
[4]	付瑞杰，周静，田风玉，焦必宁，何悦. 基于纳米材料的光学适配体传感器在农药残留检测中的应用研究进展[J]. 食品科学, 2021, 42(3): 330-338.
[5]	刘寒寒，杨书珍，李哲，张美红，彭丽桃. 碳酸铵对柑橘酸腐病菌的抑制效果及作用机制[J]. 食品科学, 2021, 42(3): 204-210.
[6]	戴尽波，沈洁，何啸峰，聂荣荣，董文静，梁沁娴. QuEChERS-超高效液相色谱-串联质谱法检测禽源性食品中氟虫腈及其代谢物[J]. 食品科学, 2021, 42(2): 325-332.
[7]	龚蕾，黄徽，韩智，江丰，彭青枝，黄宗骞，王亨. QuEChERS-UPLC-MS/MS测定果蔬中18 种琥珀酸脱氢酶抑制剂类杀菌剂[J]. 食品科学, 2021, 42(18): 261-268.
[8]	贺明阳，洪敏，王日葵，喻最新，朱莉，周炼，邓涂静. 宽皮柑橘浮皮时脱落酸积累变化及其代谢基因表达特征[J]. 食品科学, 2021, 42(17): 54-62.
[9]	钟浩文，杨国顺，陈文婷，白描，谭君. 稳定同位素内标GC-QqQ-MS/MS法测定葡萄中33 种农药残留及其污染特征分析[J]. 食品科学, 2021, 42(14): 263-269.
[10]	马丽莎，谢文平，尹怡，单奇，刘书贵，李丽春，赵成，郑光明. QuEChERS-高效液相色谱-串联质谱法测定稻田水产品中氟虫腈及其代谢物残留[J]. 食品科学, 2021, 42(14): 308-314.
[11]	高霞，陈辉，谭敏，李玉秀，何泓霖. 气相色谱-负化学源电离-质谱法测定蔬菜中氟虫腈及其代谢物残留[J]. 食品科学, 2021, 42(14): 333-338.
[12]	周若浩，吕岱竹，马晨，梁水连，相坛坛，王明月. 气相色谱-串联质谱法测定动植物源性食品中氯苯胺灵残留量[J]. 食品科学, 2021, 42(10): 311-315.
[13]	李路，李蔚，车金鑫，欧阳秋丽，陶能国. p-茴香醛抑制柑橘酸腐病菌的作用机制[J]. 食品科学, 2020, 41(9): 133-138.
[14]	梁秀美，张维一，张微，谢拾冰，何如意，徐静，苏来金，孙博伦，张井. QuEChERS-HPLC-MS/MS法同时测定水果中38 种农药的残留量[J]. 食品科学, 2020, 41(8): 288-296.
[15]	李勋兰，洪林，杨蕾，王武，韩国辉，农江飞，谭平. 11 个柑橘品种果实营养成分分析与品质综合评价[J]. 食品科学, 2020, 41(8): 228-233.

气相色谱-串联质谱法结合QuEChERS方法快速检测柑橘中52种农药多残留

Rapid Determination of 52 Pesticide Residues in Citrus by Gas Chromatography-Tandem Mass Spectrometry Coupled with QuEChER

RichHTML

PDF (PC)

可视化

摘要/Abstract

引用本文

使用本文

参考文献

相关文章 15

编辑推荐

Metrics

本文评价