气相色谱-质谱法测定荷兰豆中氟硅唑、丙环唑、苯醚甲环唑残留量
GC-MS DETERMINATION OF RESIDUAL FLUOSILAZOLE PROPICONAZOLE AND DIFENOCONAZOLE IN GREEN PEA
摘 要
试样经乙腈提取,Dual Layer ENVITM-CarbⅡ/PSA(500/500 mg)固相萃取柱净化,选择离子监测/全扫描(SIM/SCAN),同时采集气相色谱-质谱法(GC-MS)对荷兰豆中氟硅唑、丙环唑、苯醚甲环唑残留量进行定性定量分析,方法检出限分别为0.001,0.003,0.005 mg·kg-1,在0.01,0.02,0.05 mg·kg-1添加水平回收率分别为60%~120%,70%~112%,75%~110%,相对标准偏差为5.0%~12.0%.
固相萃取
SIM/SCAN同时采集
氟硅唑
丙环唑
苯醚甲环唑
荷兰豆
GC-MS
Solid-phase extraction
Synchronous SIM/SCAN data aquisition mode
Fluosilazole
Propiconazole
Difenoconazole
Green pea
Abstract
Residual amounts of fluosilazole (FSAZ),propiconazole (PPAZ) and difenoconazole (DFAZ) in green pea was determined by gas chromatography and mass spectrometry in hyphenation.The above mentioned pesticides were extracted from the sample with acetonitrile and purified by using Supelco Dual Layer ENVITM-Carb Ⅱ/PSA (500/500 mg) SPE Tube.The final extract was injected into GC for separation and followed by MS detection under EI ionization and synchronous SIM/SCAN data aquisition mode.The detection limit found for FSAZ,PPAZ and DFAZ were 0.001,0.003 and 0.005 mg·kg-1 respectively.Tests for precision and recovery were made at the concentration levels of 0.01,0.02 and 0.05 mg·kg-1,and values of RSD′s found were in the range of 5.0%-12.0%,and values of recovery were in the ranges of 60%-120%,70%-112% and 75%-110% respectively.
中图分类号 O657.37
所属栏目 工作简报
基金项目
收稿日期 2006/6/20
修改稿日期
网络出版日期
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引用该论文: WANG Lian-zhu,WANG Deng-fei,ZHENG Jun-chao,WANG Rui-long,LIU Yi-na,LIANG Ming,LU Sheng-yu. GC-MS DETERMINATION OF RESIDUAL FLUOSILAZOLE PROPICONAZOLE AND DIFENOCONAZOLE IN GREEN PEA[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2006, 42(12): 1025～1028
王连珠,王登飞,郑俊超,王瑞龙,刘溢娜,梁鸣,卢声宇. 气相色谱-质谱法测定荷兰豆中氟硅唑、丙环唑、苯醚甲环唑残留量[J]. 理化检验－化学分册, 2006, 42(12): 1025～1028
被引情况:
【1】何强,李建华,孔祥虹,乐爱山,董会生,赵洁, "固相萃取-气相色谱-质谱联用法测定食品中丙环唑残留量",理化检验－化学分册 46, 178-180(2010)
【2】陈君义,孙慧宇,王云飞, "气相色谱-串联质谱法同时测定蔬菜中4种杀菌剂残留量",理化检验－化学分册 51, 1572-1575(2015)
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参考文献
【1】李薇,冷欣夫.氟硅唑在黄瓜及土壤内残留动态研究[J].农业环境保护,2002,21(2):150-152,162．
【2】陈莉,陈家梅,夏福利,等.氟硅唑在葡萄和土壤中残留的液相色谱分析方法[J].农药学学报,2004,6(2):87．
【3】GB/T 19648-2005水果和蔬菜中446种农药多残留测定方法 气相色谱-质谱和液相色谱-串联质谱法[S]．
【4】日本厚生劳动省.食品中农用化学品残留检测方法[M].李元平,王大宁,唐英章,等译.北京:国家质检总局食品安全局、中国检验检疫科学研究院出版,2006:483-496．
【5】Julie Fillion,Ralph Hindle,Mario Lacroix,et al.Multiresidue determination of pesticides in fruit and vegetables by gas chromatography-mass-selective detection and liquid chromatography with fluorescence detection[J].Journal of AOAC International,1995,78(5):1252-1266．
【6】Julie Fillion,Francois Sauve,Jennifer Selwyn.Multiresidue method for the determination of redsidues of 251 pesticides in fruits and vegetables by gas chromatography/mass spectrometry and liquid chromatography with fluorescence detection[J].Journal of AOAC International,2000,83(3):698-713．
【7】许泓,林安清,古珑,等.果蔬中107种残留农药的气相色谱-质谱检测方法[J].分析测试学报,2004,23(3):34-38．
【8】胡小钟,储晓刚,余建新,等.气相色谱-质谱法快速筛选测定浓缩苹果汁中105种农药残留量[J].分析测试学报,2003,22(6):26-31．
【9】SN/T 1591-2005进出口茶叶中9种有机杂环类农药残留量的检测方法[S]．
【10】Darinka tajnbaher,Lucija Zupani-Kralj.Multiresidue method for determination of 90 pesticides in fresh fruits and vegetables using solid-phase extraction and gas chromatiography-mass spectrometry[J].Journal of Chromatography A,2003,1015:185-198．
【11】Eiji Ueno,Harumi Oshima,Isao Saito,et al.Multiresidue analysis of pesticides in vegetables and fruits by gas chromatography/mass spectrometry after gel permeation chromatography and graphitized carbon column cleanup[J].Journal of AOAC International,2004,87(4):1003-1015．
【12】Michelangelo Anastassiades,Steven J Lehotay,Darinka tajnbaher,et al.Fast and easy multiresidue method employing acetonitrile extracitong/partitioning and “Dispersive Solid –Phase Extraction ” for the determination of pesiticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431．
【13】黄宝勇,潘灿平,王一茹,等.气质联机分析蔬菜中农药多残留及基质效应的补偿[J].高等学校化学学报,2006,27(2):227-232．
【14】Ronald Erney D,Tina M Pawlowski,Colin F Poole.Matrix-induced peak enhancement of pesticides in gas chromatography: Is There a Solution [J].J High Resol Chromatogr,1997,20:375-378．
【15】Michelangelo Anastassiades,Katerina Matovská,Steven J Lehotay.Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides[J].Journal of Chromatography A,2003,1015:163-184．
【2】陈莉,陈家梅,夏福利,等.氟硅唑在葡萄和土壤中残留的液相色谱分析方法[J].农药学学报,2004,6(2):87．
【3】GB/T 19648-2005水果和蔬菜中446种农药多残留测定方法 气相色谱-质谱和液相色谱-串联质谱法[S]．
【4】日本厚生劳动省.食品中农用化学品残留检测方法[M].李元平,王大宁,唐英章,等译.北京:国家质检总局食品安全局、中国检验检疫科学研究院出版,2006:483-496．
【5】Julie Fillion,Ralph Hindle,Mario Lacroix,et al.Multiresidue determination of pesticides in fruit and vegetables by gas chromatography-mass-selective detection and liquid chromatography with fluorescence detection[J].Journal of AOAC International,1995,78(5):1252-1266．
【6】Julie Fillion,Francois Sauve,Jennifer Selwyn.Multiresidue method for the determination of redsidues of 251 pesticides in fruits and vegetables by gas chromatography/mass spectrometry and liquid chromatography with fluorescence detection[J].Journal of AOAC International,2000,83(3):698-713．
【7】许泓,林安清,古珑,等.果蔬中107种残留农药的气相色谱-质谱检测方法[J].分析测试学报,2004,23(3):34-38．
【8】胡小钟,储晓刚,余建新,等.气相色谱-质谱法快速筛选测定浓缩苹果汁中105种农药残留量[J].分析测试学报,2003,22(6):26-31．
【9】SN/T 1591-2005进出口茶叶中9种有机杂环类农药残留量的检测方法[S]．
【10】Darinka tajnbaher,Lucija Zupani-Kralj.Multiresidue method for determination of 90 pesticides in fresh fruits and vegetables using solid-phase extraction and gas chromatiography-mass spectrometry[J].Journal of Chromatography A,2003,1015:185-198．
【11】Eiji Ueno,Harumi Oshima,Isao Saito,et al.Multiresidue analysis of pesticides in vegetables and fruits by gas chromatography/mass spectrometry after gel permeation chromatography and graphitized carbon column cleanup[J].Journal of AOAC International,2004,87(4):1003-1015．
【12】Michelangelo Anastassiades,Steven J Lehotay,Darinka tajnbaher,et al.Fast and easy multiresidue method employing acetonitrile extracitong/partitioning and “Dispersive Solid –Phase Extraction ” for the determination of pesiticide residues in produce[J].Journal of AOAC International,2003,86(2):412-431．
【13】黄宝勇,潘灿平,王一茹,等.气质联机分析蔬菜中农药多残留及基质效应的补偿[J].高等学校化学学报,2006,27(2):227-232．
【14】Ronald Erney D,Tina M Pawlowski,Colin F Poole.Matrix-induced peak enhancement of pesticides in gas chromatography: Is There a Solution [J].J High Resol Chromatogr,1997,20:375-378．
【15】Michelangelo Anastassiades,Katerina Matovská,Steven J Lehotay.Evaluation of analyte protectants to improve gas chromatographic analysis of pesticides[J].Journal of Chromatography A,2003,1015:163-184．
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