气相色谱-离子阱-多级质谱法检测鱼体组织中19种有机氯农药

李荣; 何力; 徐进; 吴翠玲

气相色谱-离子阱-多级质谱法检测鱼体组织中19种有机氯农药

1.
中国水产科学研究院长江水产研究所,农业部淡水鱼类种质监督检验测试中心,湖北荆州434000
2.
Varian北京办事处,北京100070

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出版历程
- 收稿日期: 1899-12-31
- 修回日期: 1899-12-31
- 刊出日期: 2010-03-19

Determination of 19 Organochlorine Pesticides Residues in Fish Tissues by Gas Chromatography-Ion Trap Mass Spectrometry

1.
Yangtze River Fisheries Research Institute,Chinese Academy of Fishery Sciences,Fishery Quality Supervision and Testing Center,Ministry of Agriculture,Jingzhou 434000,China
2.
Varian office in Beijing, Beijing 100070,China

摘要

摘要: 建立了鱼体组织中19种有机氯农药残留分析的气相色谱-离子阱-多级质谱（GCIT-MS/MS）方法。试样用V（正己烷）∶V（丙酮）=1∶1溶液提取，凝胶渗透色谱和固相萃取联合净化，浓缩、定容后，上机分析。结果表明，采用EI电离模式，选择不同的监测特征离子，GC-IT-MS/MS法能灵敏测定加标试样中全部目标化合物。添加浓度为5.0 μg•kg^-1和10 μg•kg^-1时的加标回收率在76.2%～106%之间，相对标准偏差在4.8%～11%范围内；检测限（S/N=3）和定量限（S/N=10）分别为0.03～1.42 μg•kg^-1和0.1～4.27 μg•kg^-1。
- 鱼 /
- 有机氯农药 /
- 气相色谱-离子阱-多级质谱（GC-IT-MS/MS）
Abstract: A method for the simultaneous determination of 19 organochlorine pesticides(OCPs) in fish tissues was developed by gas chromatography-ion trap mass spectrometry(GC-IT-MS/MS). The samples were extracted by mixture of V (acetone)∶ V (hexane)= 1∶1 , then cleaned-up by gel permeation chromatography(GPC) and solid phase extraction(SPE), followed by analysis using GC-IT-MS/MS. The experimental results demonstrated good sensitivity for 19 target OCPs in spiked samples, by monitoring different precursor ions and product ions in electron ionization(EI) mode. Spiked reference samples are analyzed at concentration levels of 5.0 μg•kg^-1 and 10 μg•kg^-1, the average recoveries are range of 76.2%—106%, with a relative standard deviation(RSD) range of 4.8%—11%. Limits of detection(LOD) (S/N=3) are range of 0.03—1.42 μg•kg^-1. Limits of quantification(LOQ) (S/N=10) are between 0.1 μg•kg^-1 and 4.27 μg•kg^-1.
- fish /
- organochlorine pesticides /
- gas chromatography-ion trap mass spectrometry(GC-IT-MS/MS)

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参考文献(21)

[1]	WEBER K，GOERKE H. Organochlorine compounds in fish off the antarctic peninsula[J]. Chemosphere,1996, 33: 404-410.
[2]	《食品中农业化学品残留限量》编委会.食品中农业化学品残留限量:食品卷[M].北京:中国标准出版社,2006:1 563-1 603.
[3]	Informal coordination of MRLs established in Directives 76/895/EEC,86/362/EEC,86/363/EEC,and 90/642/EEC[EB/OL].http:// ec.europa.eu/food/plant/protection/resources/09-99-2.pdf.
[4]	张莹,王绪卿,赵丹宇,等.GB 2763—2005食品中农药最大残留限量[S].北京：中国标准出版社，2005.
[5]	王联珠,李晓川,孙建华,等.NY5073—2006 无公害食品水产品中有毒有害物质限量[S].北京:中国标准出版社,2005.
[6]	E YEHOUENOU A PAZOU, LAL Y P, BOKO M,et al. Contamination of fish by organochlorine pesticide residues in the ouémé river catchment in the republic of bénin[J].Environment International,2006,32(5):594-599.
[7]	ZHOU R V, ZHU L Z, KONG Q X. Persistent chlorinated pesticides in fish species from Qiantang River in East China[J]. Chemosphere,2007,68:838-847.
[8]	COELHAN M, STROHMEIER J, BARLAS H. Organochlorine levels in edible fish from the Marmara Sea，Turkey[J]. Environment International，2006，32：775-780.
[9]	MATOVSK K, LEHOTAY S J. Review practical approaches to fast gas chromatography-mass spectrometry[J].Journal of Chromatography A,2003,1 000:153-180.
[10]	庞国芳,曹彦忠,刘永明,等.GB/T 19650—2006 动物肌肉中478种农药及相关化学品残留量的测定气相色谱-质谱法[S].北京:中国标准出版社,2006.
[11]	LESUEUR C, KNITTL P, GARTNER M,et al. Analysis of 140 pesticides from conventional farming foodstuff samples after extraction with the modified QuECheRS method[J]. Food Chemistry, 2008,19: 906-914.
[12]	THANH DONG NGUYEN,EUN MI HAN,MI SUK SEO, et al. A multiresidue method for the determination of 203 pesticides in rice paddies using gas chromatography/mass spectrometry[J].Analytica Chimica Acta,2008,619:67-74.
[13]	王云凤,常春艳,陈其勇,等.凝胶渗透色谱和气相色谱-质谱法测定动物食品中27种有机氯和15种拟除虫菊酯类农药残留量[J].分析测试学报,2007,26（Sup）:253-255.
[14]	李晓娟,马晓东,佟玲.串联质谱法在农药残留分析中的应用[J].分析测试学报,2004,23（Sup）:265-266.
[15]	GARRIDO FRENICH A, MARTNEZ VIDAL J L, CRUZ SICILIA A D, et al. Multiresidue analysis of organochlorine and organophosphorus pesticides in muscle of chicken, pork and lamb by gas chromatography-triple quadrupole mass spectrometry[J]. Analytica Chimica Acta，2006，558：42-52.
[16]	FRENICH A G, BOLAOS P P, VIDAL J L M. Multiresidue analysis of pesticides in animal liver by gas chromatography using triple quadrupole tandem mass spectrometry[J].Journal of Chromatography A, 2007, 1 153: 194-202.
[17]	FANG J，WANG K X. Multiresidual analysis of organochlorine pesticides,polychlorinated biphenyls and polycyclic aromatic hydrocarbons in marine shellfishes by gas chromatography-ion trap mass spectrometry[J]. Chinese Journal of Analytical Chemistry, 2007, 35(11):1 607-1 613.
[18]	BOLAOS P P, MORENO J L F, SHTEREVA D D, et al. Development and validation of a multiresidue method for the analysis of 151 pesticide residues in strawberry by gas chromatography coupled to a triple quadrupole mass analyzer[J]. Rapid Commun Mass Spectrom, 2007,21: 2 282-2 294.
[19]	SCHACHTERLE S, FEIGEL C. Pesticide residue analysis in fresh produce by gas chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 1996, 754: 411-422.
[20]	FERNNDEZ MORENO J L, ARREBOLA LIBANAS F J， GARRIDO A, et al. Evaluation of different sample treatments for determining pesticide residues in fat vegetable matrices like avocado by low-pressure gas chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 2006, 1 111: 97-105.
[21]	FIDALGO-USED N， BLANCO-GONZLEZ E， SANZ-MEDEL A. Sample handling strategies for the determination of persistent trace organic contaminants from biota samples[J]. Analytica Chimica Acta, 2007, 590: 1-16.

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气相色谱-离子阱-多级质谱法检测鱼体组织中19种有机氯农药

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出版历程

Determination of 19 Organochlorine Pesticides Residues in Fish Tissues by Gas Chromatography-Ion Trap Mass Spectrometry

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出版历程

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