GC-MS/MS Determination of Residual Amounts of Pesticides in Ginger
摘 要
采用气相色谱-串联质谱法测定生姜中25种农药的残留量。样品用乙腈提取,过NH2/Carbon固相萃取柱净化,将淋出液浓缩后用正己烷-丙酮(9+1)溶液定容。通过VF-5MS色谱柱分离,串联质谱测定。25种农药的质量浓度在0.020~0.500 mg·L-1范围内与其峰面积均呈线性关系,检出限(3S/N)在0.2~10.0 μg·kg-1之间。加入两个浓度水平的农药标准溶液进行了回收试验,多数农药的回收率在77%~130%之间,相对标准偏差(n=5)均小于20%。
Abstract
Gas chromatography in hyphenation with tandem mass spectrometry (GC-MS/MS) was applied to the determination of residual amounts of 25 pesticides in ginger. The sample was extracted with acetonitrile, which was concentrated and purified by NH2/Carbon solid-phase extraction column. The eluate was evaporated to near dryness and diluted to a definite volume with mixture of n-hexane and acetone (9+1), and separated on the VF-5MS column. The eluate was used for tandem MS analysis. Linear relationships between values of peak area and mass concentration of the 25 pesticides were obtained in the same range of 0.020-0.500 mg·L-1, with detection limits (3S/N) in the range of 0.2-10.0 μg·kg-1. Test for recovery were made by addition of standard at 2 different concentration levels, values of recovery for most of the pesticides found were in the range of 77%-130%, with values of RSD′s (n=5) less than 20%.
中图分类号 O657.63
所属栏目 工作简报
基金项目
收稿日期 2011/2/27
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备注易盛国(1955-),男,四川成都人,副研究员,主要从事食品中农药残留分析。
引用该论文: YI Sheng-guo,HOU Xue,HAN Mei,YANG Xiao-feng. GC-MS/MS Determination of Residual Amounts of Pesticides in Ginger[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2012, 48(5): 534~537
易盛国,侯雪,韩梅,杨晓凤. 气相色谱-串联质谱法测定生姜中25种农药残留量[J]. 理化检验-化学分册, 2012, 48(5): 534~537
被引情况:
【1】张莉,徐万邦,蒋忠军, "毛细管气相色谱法测定沉香中20种有机氯农药残留量",理化检验-化学分册 50, 987-990(2014)
【2】王海凤,刘海学,王俊斌,郭宏,王瑞, "气相色谱-质谱法测定高粱籽粒中11种有机磷农药残留量",理化检验-化学分册 49, 651-653(2013)
【3】曹艳平,杨路平,邵立君, "气相色谱-质谱法测定茶叶中23种农药残留量",理化检验-化学分册 51, 647-650(2015)
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参考文献
【1】ANASTASSIADES M, LEHOTAY S J, TAJNBAHER D, et. al. Fast and easy multiresidue method employing acetonitrile extraction/partitioning and “dispersive solid-phase extraction” for the determination of pesticide residues in produce[J]. AOAC Int, 2003,86:412-431.
【2】LEHOTAY S J, DE KOK A, HIEMSTRA M. Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection[J]. AOAC Int, 2005,88:595-614.
【3】LEHOTAY S J, MASTOVSKA K, LISHFIELD A R. Use of buffering to improve resuits of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables[J]. AOAC Int, 2005,88:615-629.
【4】王建华,徐强,焦奎,等.蔬菜中有机氯农药残留的超临界流体提取和气相色谱法测定[J].色谱, 1998,16(6):506-510.
【5】CHU Xiao-gang, HU Xiao-zhong, YAO Hui-yuan. Determination of 266 pesticide residues in apple juice by matrix solid-phase dispersion and gas chromatography-mass selective detection[J]. Journal of Chromatography A, 2005,1063:201-210.
【6】FERNNDEZ M, PIC Y, MANES J. Determination of carbamate residues in fruits and vegetables by matrix solid-phase dispersion and liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2000,871:43-56.
【7】蔡亚岐,刘稷燕,江桂斌.固相微萃取-液相色谱联用技术研究进展[J].化学进展, 2004,16(5):708-715.
【8】GFRERER M, LANKMAYR E. Screening, optimization and validation of microwave-assisted extraction for the determination of persistent organochlorine pesticides[J]. Analytica Chimica Acta, 2005,533:203-211.
【2】LEHOTAY S J, DE KOK A, HIEMSTRA M. Validation of a fast and easy method for the determination of residues from 229 pesticides in fruits and vegetables using gas and liquid chromatography and mass spectrometric detection[J]. AOAC Int, 2005,88:595-614.
【3】LEHOTAY S J, MASTOVSKA K, LISHFIELD A R. Use of buffering to improve resuits of problematic pesticides in a fast and easy method for residue analysis of fruits and vegetables[J]. AOAC Int, 2005,88:615-629.
【4】王建华,徐强,焦奎,等.蔬菜中有机氯农药残留的超临界流体提取和气相色谱法测定[J].色谱, 1998,16(6):506-510.
【5】CHU Xiao-gang, HU Xiao-zhong, YAO Hui-yuan. Determination of 266 pesticide residues in apple juice by matrix solid-phase dispersion and gas chromatography-mass selective detection[J]. Journal of Chromatography A, 2005,1063:201-210.
【6】FERNNDEZ M, PIC Y, MANES J. Determination of carbamate residues in fruits and vegetables by matrix solid-phase dispersion and liquid chromatography-mass spectrometry[J]. Journal of Chromatography A, 2000,871:43-56.
【7】蔡亚岐,刘稷燕,江桂斌.固相微萃取-液相色谱联用技术研究进展[J].化学进展, 2004,16(5):708-715.
【8】GFRERER M, LANKMAYR E. Screening, optimization and validation of microwave-assisted extraction for the determination of persistent organochlorine pesticides[J]. Analytica Chimica Acta, 2005,533:203-211.
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