液相色谱-串联质谱法测定蔬菜、水果中氨基甲酸酯类农药残留量
LC-MS/MS Determination of Residual Amounts of Carbamate Pesticides in Vegetables and Fruits
摘 要
应用液相色谱-串联质谱法测定了蔬菜及水果中10种氨基甲酸酯类农药的残留量.试样用乙腈提取,提取液经转变成甲醇-二氯甲烷(1+99)溶液后用固相萃取法净化.淋出液经氮气吹干后,用1 mL乙腈溶解残渣,所得溶液用于LC-MS/MS测定.测定中用C18色谱柱固定相,用乙腈及甲醇-水溶液以不同比例混合后作为流动相进行梯度淋洗.10种农药的检出限(3S/N)均为1 μg·kg-1.在3种不同的浓度水平上(1,10,100 μg·kg-1)作回收试验,测得椰菜中农药的回收率在78.5%~105.0%之间,橙中农药的回收率在80.3%~106.0%之间,相应测定结果的相对标准偏差(n=6)依次在4.6%~19.8%及3.5%~17.7%范围内.
氨基甲酸酯类农药
蔬菜
水果
LC-MS/MS
Carbamate pesticides
Vegetables
Fruits
Abstract
Residual amounts of ten carbamate pesticides in vegetables and fruits were determined by LC-MS/MS.Samples of vegetables or fruits were extracted with acetonitrile.Sample solution in CH3OH-CH2Cl2(1+99) was purified by SPE and the eluate,after evaporation to near dryness by N2-blowing and dissolution in 1 mL of acetonitrile,was used for LC-MS/MS determination,with C18 chromatographic column and gradient elution using acetonitrile and methanol-water mixed solution as mobile phase.Detection limits (3S/N) for the 10 pesticides found were 1 μg·kg-1.Recovery of the method was tested at 3 concentration levels of 1,10,100 μg·kg-1 for each of the 10 pesticides,values of recovery found for savoy were ranged from 78.5% to 105.0% and for orange were ranged from 80.3% to 106.0%,with values of RSD′s (n=6) in the ranges of 4.6%-19.8% and 3.5%-17.7% respectively.
中图分类号 O657.63
所属栏目 工作简报
基金项目
收稿日期 2008/1/9
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备注罗惠明(1964-),女,广东人,副主任医师,主要从事进出口食品卫生监督检验工作.
引用该论文: LUO Hui-ming,CHEN Yan-qin,LIANG Xi-yang,ZHANG Lin-tian. LC-MS/MS Determination of Residual Amounts of Carbamate Pesticides in Vegetables and Fruits[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2009, 45(8): 994～997
罗惠明,陈燕勤,梁希扬,张林田. 液相色谱-串联质谱法测定蔬菜、水果中氨基甲酸酯类农药残留量[J]. 理化检验－化学分册, 2009, 45(8): 994～997
被引情况:
【1】何华丽,徐小民,周珊,莫卫民,任一平, "液相色谱-串联质谱法测定桃中31种农药残留",理化检验－化学分册 50, 1351-1356(2014)
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参考文献
【1】贾微,王磊石,赵雷,等.气相色谱-质谱法同时检测七种氨基甲酸酯类杀虫剂[J].中国卫生检验杂志,2003,13(2):205-206．
【2】刘敏,端裕树,宋苑苑,等.分散固相萃取-液相色谱-质谱法检测蔬菜水果中氨基甲酸酯和有机磷农药[J].分析化学,2006,34(7):941-945．
【3】李英,周艳明,牛森,等.蔬菜、水果中氨基甲酸酯类农药多残留分析方法的研究[J].现代科学仪器,2005,6:68-70．
【4】韩梅,易盛国,张义蓉,等.蔬菜中有机磷和氨基甲酸酯类农药残留的气相色谱测定方法探讨[J].分析试验室,2003,22(增刊):187-190．
【5】LIU M,Hashi Y,Song,Y Y,et al.Simultaneous determination of carbamate and organophosphorus pesticides infruits and vegetables by liquid chromatography-mass spectrometry[J].Journal of Chromatography A,2005,1097(1/2):183-187．
【6】陈笑梅,胡贝贞,刘海山,等.高效液相色谱-串联质谱法测定粮谷中9种氨基甲酸酯类农药残留[J].分析化学,2007,35(1):106-110．
【7】王明泰,牟峻,吴剑,等.蔬菜及水果中77种有机磷和氨基甲酸酯农药残留量检测技术研究[J].食品科学,2007,28(3):247-253．
【8】TOMOMI G,YUKO I,HISAO O,et al.The high throughput analysis of N-methyl carbamate pesticides in wine andjuice by electrospray ionization liquid chromatography tandem mass spectrometry with direct sampleinjection into a short column[J].Anal Chim Acta,2005,531(1):79-86．
【9】TOMOMI G,YUKO I,SADAJI Y,et al.The high throughput analysis of N-methyl carbamate pesticides in fruits andvegetables by liquid chromatography electrospray ionization tandem mass spectrometry using a shortcolumn[J].Anal Chim Acta,2006,555(2):225-232．
【10】KAWASAKI M,INOUE T,FUKUHARA K,et al.Study on GC/MS (SIM) for determination of carbamate and organonitrogenpesticides in foods with simple clean-up by SPE method[J].食品卫生学杂志,1999,40(5):382-390．
【11】高玲,杨元,王炼,等.气相色谱-质谱法同时测定水中7种氨基甲酸酯类杀虫剂[J].中国卫生检验杂志,2005,15(6):713-714．
【12】杨大进,张莹,方从容.大米中有机磷和氨基甲酸酯农药残留毛细管气相色谱测定法[J].卫生研究,1994,23(2):97-100．
【13】杨红,陈如东,朱红梅,等.紫甘蓝中氨基甲酸酯类农药多残留分析方法研究[J].南京农业大学学报,2005,28(1):103-106．
【2】刘敏,端裕树,宋苑苑,等.分散固相萃取-液相色谱-质谱法检测蔬菜水果中氨基甲酸酯和有机磷农药[J].分析化学,2006,34(7):941-945．
【3】李英,周艳明,牛森,等.蔬菜、水果中氨基甲酸酯类农药多残留分析方法的研究[J].现代科学仪器,2005,6:68-70．
【4】韩梅,易盛国,张义蓉,等.蔬菜中有机磷和氨基甲酸酯类农药残留的气相色谱测定方法探讨[J].分析试验室,2003,22(增刊):187-190．
【5】LIU M,Hashi Y,Song,Y Y,et al.Simultaneous determination of carbamate and organophosphorus pesticides infruits and vegetables by liquid chromatography-mass spectrometry[J].Journal of Chromatography A,2005,1097(1/2):183-187．
【6】陈笑梅,胡贝贞,刘海山,等.高效液相色谱-串联质谱法测定粮谷中9种氨基甲酸酯类农药残留[J].分析化学,2007,35(1):106-110．
【7】王明泰,牟峻,吴剑,等.蔬菜及水果中77种有机磷和氨基甲酸酯农药残留量检测技术研究[J].食品科学,2007,28(3):247-253．
【8】TOMOMI G,YUKO I,HISAO O,et al.The high throughput analysis of N-methyl carbamate pesticides in wine andjuice by electrospray ionization liquid chromatography tandem mass spectrometry with direct sampleinjection into a short column[J].Anal Chim Acta,2005,531(1):79-86．
【9】TOMOMI G,YUKO I,SADAJI Y,et al.The high throughput analysis of N-methyl carbamate pesticides in fruits andvegetables by liquid chromatography electrospray ionization tandem mass spectrometry using a shortcolumn[J].Anal Chim Acta,2006,555(2):225-232．
【10】KAWASAKI M,INOUE T,FUKUHARA K,et al.Study on GC/MS (SIM) for determination of carbamate and organonitrogenpesticides in foods with simple clean-up by SPE method[J].食品卫生学杂志,1999,40(5):382-390．
【11】高玲,杨元,王炼,等.气相色谱-质谱法同时测定水中7种氨基甲酸酯类杀虫剂[J].中国卫生检验杂志,2005,15(6):713-714．
【12】杨大进,张莹,方从容.大米中有机磷和氨基甲酸酯农药残留毛细管气相色谱测定法[J].卫生研究,1994,23(2):97-100．
【13】杨红,陈如东,朱红梅,等.紫甘蓝中氨基甲酸酯类农药多残留分析方法研究[J].南京农业大学学报,2005,28(1):103-106．
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