超高效液相色谱-串联质谱法测定莲雾中51种农药残留量
UPLC-MS/MS Determination of 51 Pesticide Residues in Syzygium Samarangense
摘 要
莲雾样品用含1%（体积分数）乙酸的乙腈提取后，经多壁碳纳米管滤过型净化柱净化，采用超高效液相色谱-串联质谱法测定其中51种农药的残留量。质谱分析中采用电喷雾离子源和多反应监测模式。结果表明：51种农药的质量浓度在0.005~0.2 mg·L-1内与其峰面积呈线性关系，检出限（3S/N）为0.06~1.50 μg·kg-1。按标准加入法进行回收试验，回收率为60.4%~120%，测定值的相对标准偏差（n=6）为2.0%~16%。
多壁碳纳米管滤过型净化
莲雾
农药残留
UPLC-MS/MS
multiplug filtration clean-up with multiwalled carbon nanotube
Syzygium samarangense
pesticide residue
Abstract
The sample of Syzygium samarangense was extracted with acetonitrile containing 1% (φ) acetic acid, and cleaned up with multiplug filtration using multiwalled carbon nanotubes, and the 51 pesticide residues were determined by UPLC-MS/MS. ESI and MRM were adopted in MS analysis. As shown by the results, linear relationships between values of peak area and mass concentration of 51 pesticide residues were found in the same range of 0.005-0.2 mg·L-1, and detection limits (3S/N) ranged from 0.06 to 1.50 μg·kg-1. Test for recovery was made by standard addition method, giving results in the range of 60.4%-120%, and RSDs (n=6) ranged from 2.0% to 16%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201810003
所属栏目 试验与研究
基金项目 海南省自然科学基金项目（SQ2018QNJJ0014）；热带农产品质量安全科技创新团队项目（1630082017002）
收稿日期 2017/10/22
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备注乐渊,助理研究员,研究方向为农产品质量安全,leyuan06@sina.com
引用该论文: LE Yuan,LIU Chunhua,ZHANG Zhenshan,LI Chunli. UPLC-MS/MS Determination of 51 Pesticide Residues in Syzygium Samarangense[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(10): 1129～1137
乐渊,刘春华,张振山,李春丽. 超高效液相色谱-串联质谱法测定莲雾中51种农药残留量[J]. 理化检验－化学分册, 2018, 54(10): 1129～1137
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参考文献
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【16】BS EN 15662:2008 Foods of plant origin——Determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by Dispersive SPE-QuEChERS-method[S].
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【18】刘进玺,秦珊珊,冯书惠,等.高效液相色谱-串联质谱法测定食用菌中农药多残留的基质效应[J].食品科学, 2016,37(18):171-177.
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【20】MARTINEZ G M, LOPEZ L T, GIL G M, et al. A comparative study of the correction of systematic errors in the quantitation of pyrethroids in vegetables using calibration curves prepared using standards in pure solvent[J]. Analytical and Bioanalytical Chemistry, 2003,375(5):653-660.
【2】林庆光,陶挺燕,符碧海.莲雾产期调控技术[J].热带农业工程, 2013,37(3):25-27.
【3】杨凤珍,李敏,高兆银,等.莲雾果实病害及防治研究进展[J].浙江农业科学, 2009(5):961-964.
【4】车建美,刘波,阮传清,等.莲雾黑腐病病原菌的鉴定及其生物学特性研究[J].福建农业学报, 2014,29(6):580-585.
【5】GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].
【6】ANASTASSUADE M, LEHOTAY S J, STAJNBAHER 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]. Journal of AOAC International, 2003,86(2):412-431.
【7】OZGUR G, BULENT K. Evaluation of QuEChERS sample preparation and liquid chromatography-triple-quadrupole mass spectrometry method for the determination of 109 pesticide residues in tomatoes[J]. Food Chemistry, 2015,176:319-332.
【8】HAN Y, ZOU N, SONG L, et al. Simultaneous determination of 70 pesticide residues in leek, leaf lettuce and garland chrysanthemum using modified QuEChERS method with multi-walled carbon nanotubes as reversed-dispersive solid-phase extraction materials[J]. Journal of Chromatography B, 2015,1005:56-64.
【9】MACHADO I, GEREZ N, PISTON M, et al. Determination of pesticide residues in globe artichoke leaves and fruits by GC-MS and LC-MS/MS using the same QuEChERS procedure[J]. Food Chemistry, 2017,227:227-236.
【10】WU C C. Multiresidue method for the determination of pesticides in Oolong tea using QuEChERS by gas chromatography-triple quadrupole tandem mass spectrometry[J]. Food Chemistry, 2017,229:580-587.
【11】马立利,贾丽,周欣燃,等.多壁碳纳米管滤过型净化柱净化-超高效液相色谱/串联质谱法同时测定生姜中的涕灭威及其代谢物[J].色谱, 2014,32(6):635-639.
【12】ZHAO P Y, HUANG B Y, LI Y J, et al. Rapid multiplug filtration cleanup with multiple-walled carbon nanotubes and gas chromatography-triple-quadruple mass spectrometry detection for 186 pesticide residues in tomato and tomato products[J]. Journal of Agricultural and Food Chemistry, 2014,62(17):3710-3725.
【13】ZOU N, HAN Y T, LI Y J, et al. Multiresidue method for determination of 183 pesticide residues in leeks by rapid multiplug filtration cleanup and gas chromatography-tandem mass spectrometry[J]. Journal of Agricultural and Food Chemistry, 2016,64(31):6061-6070.
【14】潘灿平,赵鹏跃.一种农药残留的净化方法及其专用净化器:201210586885.9[P]. 2012-12-28.
【15】LEHOTY S J, MARY O N, JOSE T, et al. Determination of pesticide residues in foods by acetonitrile extraction and partitioning with magnesium sulfate:Collaborative study[J]. Journal of AOAC International, 2007,90(2):485-520.
【16】BS EN 15662:2008 Foods of plant origin——Determination of pesticide residues using GC-MS and/or LC-MS/MS following acetonitrile extraction/partitioning and clean-up by Dispersive SPE-QuEChERS-method[S].
【17】李杨梅,杨敏,谭伟,等.多壁碳纳米管固相萃取-气相色谱法检测蔬菜中毒死蜱、丙溴磷和三唑磷农药残留[J].食品工业科技, 2014,35(19):316-320.
【18】刘进玺,秦珊珊,冯书惠,等.高效液相色谱-串联质谱法测定食用菌中农药多残留的基质效应[J].食品科学, 2016,37(18):171-177.
【19】GARRIDO F A, MARTINEZ J L, FERNANDEZ M J, et al. Compensation for matrix effects in gas chromatography-tandem mass spectrometry using a single point standard addition[J]. Journal of Chromatography A, 2009,1216(23):4798-4808.
【20】MARTINEZ G M, LOPEZ L T, GIL G M, et al. A comparative study of the correction of systematic errors in the quantitation of pyrethroids in vegetables using calibration curves prepared using standards in pure solvent[J]. Analytical and Bioanalytical Chemistry, 2003,375(5):653-660.
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