固相萃取-在线凝胶渗透色谱-气相色谱-质谱法测定豆芽中53种农药残留量
GC-MS Determination of Residual Amounts of 53 Pesticides in Bean Sprout with Online Gel Permeation Chromatography and Solid-Phase Extraction
摘 要
采用固相萃取-在线凝胶渗透色谱-气相色谱-质谱法测定豆芽中53种农药残留量.豆芽样品以乙酸-乙腈(1+99)混合液提取,固相萃取小柱净化,采用在线凝胶渗透色谱-气相色谱分离,在质谱分析中采用选择离子监测模式.53种农药的质量浓度均在0.01~1.0 mg·L-1范围内与其峰面积呈线性关系,方法的检出限在0.1~6.0 μg·kg-1之间.在20,50,100 μg·kg-1等3个浓度水平进行加标回收试验,回收率在72.3%~104%之间,测定值的相对标准偏差(n=6)在1.6%~6.6%之间.
农药
豆芽
在线凝胶渗透色谱
固相萃取
GC-MS
Pesticides
Bean sprout
Online gel permeation chromatography
Solid-phase
Abstract
GC-MS was applied to the determination of residual amounts of 53 pesticides in bean sprout with online gel permeation chromatography and solid-phase extraction. The bean sprout sample was extracted with the mixture of acetic acid-acetonitrile (1+99),and purified with solid-phase extraction column. Online gel permeation chromatography and GC was used for separation and the selected ion monitoring mode was adopted in MS determination. Linear relationships between values of peak area and mass concentration of the 53 pesticides were kept in the same range of 0.01-1.0 mg·L-1,with detection limits in the range of 0.1-6.0 μg·kg-1. Tests for recovery were made by standard addition method at the concentration levels of 20,50,100 μg·kg-1,giving values of recovery and RSD′s (n=6) in the ranges of 72.3%-104% and 1.6%-6.6%,respectively.
中图分类号 O657.63
所属栏目 试验与研究
基金项目 中国热带农业科学院院本级基金(1630062013012)
收稿日期 2014/3/7
修改稿日期
网络出版日期
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备注程盛华(1980-),男,江西九江人,助理研究员,硕士研究生,研究方向为食品安全与检测.
引用该论文: CHENG Sheng-hua,ZHANG Li-qiang,WEI Xiao-yi,WU Hao,LI Ji-hua. GC-MS Determination of Residual Amounts of 53 Pesticides in Bean Sprout with Online Gel Permeation Chromatography and Solid-Phase Extraction[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2015, 51(2): 146～152
程盛华,张利强,魏晓奕,吴浩,李积华. 固相萃取-在线凝胶渗透色谱-气相色谱-质谱法测定豆芽中53种农药残留量[J]. 理化检验－化学分册, 2015, 51(2): 146～152
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参考文献
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【12】田绍琼,毛秀红,苗水,等.气相色谱-串联质谱法测定人参和黄芪中7种毒杀芬残留量[J].色谱,2012,30(1):14-20.
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【14】韩笑,娄喜山,张莉,等.基质固相分散-超高效液相色谱-串联质谱法检测蔬菜中残留的苯甲酰脲类和双酰肼类杀虫剂[J].色谱,2010,28(4):341-347.
【15】刘建军.超高效液相色谱-串联质谱法测定大米中34种有机含磷农药残留量[J].理化检验-化学分册,2012,48(10):1167-1170.
【2】SCHENCK F J,HOBBS J E. Evaluation of the quick,easy,cheap,effective,rugged,and safe (QuEChERS) approach to pesticide residue analysis[J]. Bull Environ Contam Toxicol,2004,73(1):24-30.
【3】HERCEGOVA,KRUZ D,MATISOV E. Comparison of sample preparation methods combined with fast gas chromatography-mass spectrometry forultratrace analysis of pesticide residues in baby food[J]. J Sep Sci,2006,29(8):1102-1109.
【4】LIU Li-bin,HASHI Y,QIN Ya-ping,et al. Development of automated online gel permeation chromatography gas chromatograph mass spectrometry for measuring multiresidual pesticides in agricultural products[J]. Journal of Chromatography B,2007,845(1):61-68.
【5】SCHENZLER C,THEIR H P. European standardization of methods for pesticide residue analysis in foods-current status[J]. Food Additives and Contaminants,2001,18(10):875-879.
【6】Syoku-An No. 0124001Analytical methods for residual compositional substances of agricultural chemicals,feed additives,and veterinary drugs in food［S］.
【7】LU Da-sheng,QIU Xin-lei,FENG Chao,et al. Simultaneous determination of 45 pesticides in fruit and vegetable using an improved QuEChERS method and on-line gel permeation chromatography gas chromatography mass spectrometer[J]. Journal of Chromatography B,2012,845(1):17-21.
【8】卢大胜,邱欣磊,林元杰,等.QuEChERS方法联合GPC-GCMS测定蔬菜水果中农药残留中的应用[J].质谱学报,2011,32(4):229-235.
【9】NY/T 761-2008蔬菜和水果中有机磷、有机氯、拟除虫菊酯和氨基甲酸酯类农药多残留的测定［S］.
【10】阮华,荣维广,马永健,等.QuEChERS-在线凝胶色谱-气相色谱-质谱法测定大米、黍子和小麦中34种农药残留[J].色谱,2013,31(12):1211-1217.
【11】陈红平,刘新,汪庆华,等.气相色谱-串联质谱法测定茶叶中88种农药残留量[J].色谱,2011,29(5):409-416.
【12】田绍琼,毛秀红,苗水,等.气相色谱-串联质谱法测定人参和黄芪中7种毒杀芬残留量[J].色谱,2012,30(1):14-20.
【13】CAPPELINI L T D,CORDEIRO D,BRONDI S H G,et al. Development of methodology for determination of pesticides residue in water by SPE/HPLC/DAD[J]. Environmental Technology,2012,33(20):2299-2304.
【14】韩笑,娄喜山,张莉,等.基质固相分散-超高效液相色谱-串联质谱法检测蔬菜中残留的苯甲酰脲类和双酰肼类杀虫剂[J].色谱,2010,28(4):341-347.
【15】刘建军.超高效液相色谱-串联质谱法测定大米中34种有机含磷农药残留量[J].理化检验-化学分册,2012,48(10):1167-1170.
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