QuEChERS法结合气相色谱-质谱法同时测定葡萄酒中16种农药残留
Determination of 16 Pesticide Residues in Wine by GC-MS Combined with QuEChERS
摘 要
采用气相色谱-质谱法(GC-MS)测定葡萄酒中有机磷类及有机氯类等16种农药残留。样品经酸化乙腈提取后,提取液采用QuEChERS前处理法,经N-丙基乙二胺-石墨化碳黑-C18粉末净化。净化液采用Agilent HP-5MS色谱柱分离,质谱中采用电子轰击离子源-选择离子监测模式。16种农药的线性范围为0.05~2.00 mg·L-1,方法的检出限(3S/N)在0.006~0.060 mg·kg-1之间。对空白样品进行加标回收试验,回收率在87.6%~105%之间,测定值的相对标准偏差(n=6)在0.77%~6.9%之间。方法可以用于葡萄酒中农药残留的进出口检测。
QuEChERS法
农药残留
葡萄酒
GC-MS
QuEChERS
Pesticide residues
Wine
Abstract
A method of GC-MS coupled with QuEChERS was applied for simultaneous determination of 16 kinds of pesticide residues in wine. The sample was extracted with acidified acetonitrile. The extract was purified by QuEChERS method, using the mixture of N-propylethylenediamine, graphitized carbon black and C18 powder, and then separated on an Agilent HP-5MS column and detected by MS adopting EI-SIM. The linearity range of the mass concentration of 16 kinds of pesticides was 0.05-2.00 mg·L-1 with detection limits in the range of 0.006-0.060 mg·kg-1. Tests for recovery were made by standard addition method, giving values of recovery in the range of 87.6%-105%, and RSD (n=6) in the range of 0.77%-6.9%. The method was used for analysis of pesticide residues in wine samples for import and export inspection.
中图分类号 O657.63
所属栏目 工作简报
基金项目 国家质检总局科研项目(2013IK187)
收稿日期 2014/5/5
修改稿日期
网络出版日期
作者单位点击查看
联系人作者粟智(suzhixj@sina.com)
备注冯然军(1987-),男,河南濮阳人,硕士研究生,主要从事人体运动科学研究。
引用该论文: FENG Ran-jun,SU Zhi,LIU Jun. Determination of 16 Pesticide Residues in Wine by GC-MS Combined with QuEChERS[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(4): 480～484
冯然军,粟智,刘俊. QuEChERS法结合气相色谱-质谱法同时测定葡萄酒中16种农药残留[J]. 理化检验－化学分册, 2015, 51(4): 480～484
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参考文献
【1】朱学良,戚向阳,岳晶念,等.基质固相分散气相色谱电子捕获检测器测定葡萄酒中5种农药残留［J］.分析化学, 2007,35(2):259-262.
【2】SHARMA D, NAGPAL A, PAKADE Y B, et al. Analytical methods for estimation of organophosphorus pesticide residues in fruits and vegetables: a review［J］. Talanta, 2010,82(4):1077-1089.
【3】陈珠灵,陈飞,陈红青.高效液相色谱法测定蔬菜中3种有机磷农药残留量［J］.福州大学学报:自然科学版, 2005,33(1):98-100.
【4】刘庆斌,张睿,王海涛,等.高效液相色谱串联质谱法对栀子中11种有机磷农药残留的检测［J］.分析测试学报, 2010(1):73-76.
【5】王连珠,周昱,陈泳,等.QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估［J］.色谱, 2012,30(2):146-153.
【6】王敏,韩芳,张蕾,等.高效液相色谱-串联质谱同位素内标法测定茶叶中25种有机磷农药残留［J］.分析试验室, 2013,32(4):76-81.
【7】朱莉萍,曲坤,朱涛,等.液相色谱-串联质谱法测定蔬菜及其制品中5种农药残留量［J］.理化检验-化学分册, 2014,50(5):551-554.
【8】王兴宁,蔡秋,刘康书,等.气相色谱-串联质谱法测定烟草中97种农药残留量［J］.理化检验-化学分册, 2014,50(2):1561-1566.
【9】林慧纯,胡祥娜,禹绍周.蔬菜中杀扑磷农药残留的气相色谱-串联质谱法测定的新方法研究［J］.湖南农业科学, 2012(2):71-72.
【10】SALVADOR I M, FRENICH A G, GONZALEZ F E, et al. Determination of organophosphorus pesticides in vegetables by GC with pulsed flame-photometric detection, and confirmation by MS［J］. Chromatographia, 2006,64(11/12):667-672.
【11】韩梅,杨晓凤,侯雪,等.凝胶渗透色谱净化-气相色谱法测定酱腌菜中多种有机磷农药残留［J］.西南农业学报, 2012,24(6):2363-2368.
【12】王迪,刘潇威,刘岩,等.蔬菜、水果中12种限量有机磷农药残留量测定方法［J］.分析试验室, 2010,29(7):37-41.
【2】SHARMA D, NAGPAL A, PAKADE Y B, et al. Analytical methods for estimation of organophosphorus pesticide residues in fruits and vegetables: a review［J］. Talanta, 2010,82(4):1077-1089.
【3】陈珠灵,陈飞,陈红青.高效液相色谱法测定蔬菜中3种有机磷农药残留量［J］.福州大学学报:自然科学版, 2005,33(1):98-100.
【4】刘庆斌,张睿,王海涛,等.高效液相色谱串联质谱法对栀子中11种有机磷农药残留的检测［J］.分析测试学报, 2010(1):73-76.
【5】王连珠,周昱,陈泳,等.QuEChERS样品前处理-液相色谱-串联质谱法测定蔬菜中66种有机磷农药残留量方法评估［J］.色谱, 2012,30(2):146-153.
【6】王敏,韩芳,张蕾,等.高效液相色谱-串联质谱同位素内标法测定茶叶中25种有机磷农药残留［J］.分析试验室, 2013,32(4):76-81.
【7】朱莉萍,曲坤,朱涛,等.液相色谱-串联质谱法测定蔬菜及其制品中5种农药残留量［J］.理化检验-化学分册, 2014,50(5):551-554.
【8】王兴宁,蔡秋,刘康书,等.气相色谱-串联质谱法测定烟草中97种农药残留量［J］.理化检验-化学分册, 2014,50(2):1561-1566.
【9】林慧纯,胡祥娜,禹绍周.蔬菜中杀扑磷农药残留的气相色谱-串联质谱法测定的新方法研究［J］.湖南农业科学, 2012(2):71-72.
【10】SALVADOR I M, FRENICH A G, GONZALEZ F E, et al. Determination of organophosphorus pesticides in vegetables by GC with pulsed flame-photometric detection, and confirmation by MS［J］. Chromatographia, 2006,64(11/12):667-672.
【11】韩梅,杨晓凤,侯雪,等.凝胶渗透色谱净化-气相色谱法测定酱腌菜中多种有机磷农药残留［J］.西南农业学报, 2012,24(6):2363-2368.
【12】王迪,刘潇威,刘岩,等.蔬菜、水果中12种限量有机磷农药残留量测定方法［J］.分析试验室, 2010,29(7):37-41.
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