LC-MS/MS Determination of Residual Amounts of 5 Neonicotinoid Pesticides in Tea with Dispersive Solid Phase Extraction Using Multiwalled Carbon Nanotubes as Adsorbent
摘 要
采用多壁碳纳米管分散固相萃取-液相色谱-串联质谱法测定茶叶中啶虫脒、噻虫胺、吡虫啉、噻虫啉、噻虫嗪等5种烟碱类农药的残留量。粉碎后的茶叶样品用水浸泡30 min后,用乙腈提取,以多壁碳纳米管作为吸附剂去除杂质。以Agilent C18色谱柱为分离柱,以不同体积比的5 mmol·L-1乙酸铵-0.1%(体积分数)甲酸溶液和甲醇的混合液为流动相进行梯度洗脱,采用电喷雾正离子源和多反应监测模式检测。5种烟碱类农药的质量浓度均在1.0~20 μg·L-1内与其对应的峰面积呈线性关系,测定下限(10S/N)均为0.01 mg·kg-1。以空白样品为基体进行加标回收试验,所得回收率为80.5%~98.7%,测定值的相对标准偏差(n=6)为5.0%~13%。
Abstract
LC-MS/MS was applied to the determination of residual amounts of 5 neonicotinoid pesticides, i.e. acetamprid,clothiaindin,imidacloprid, thiacloprid and thiamethoxam in tea with dispersive solid phase extraction using multiwalled carbon nanotubes as adsorbent. The tea sample after comminution was immersed with water for 30 min, and then extracted with acetonitrile. Multiwalled carbon nanotubes were used as adsorbent to remove impurities. Agilent C18 chromatographic column was used as stationary phase, and the mixture of 5 mmol·L-1 ammonium acetate-0.1% (φ) formic acid solution and methanol mixed in different ratios was used as mobile phase in gradient elution. ESI+ and multi-reactions monitor mode were adopted in MS/MS. Linear relationships between values of peak area and mass concentration of the 5 neonicotinoid pesticides were kept in the same range of 1.0-20 μg·L-1, with the same lower limit of determination (10S/N) of 0.01 mg·kg-1. On the base of blank sample, test for recovery was made by standard addition method; values of recovery found were in the range of 80.5%-98.7%, with RSD's (n=6) in the range of 5.0%-13%.
中图分类号 O657.63 DOI 10.11973/lhjy-hx201805021
所属栏目 专题报道(食品分析)
基金项目 国家质检总局科技计划项目(2015IK302);浙江省分析测试项目(2016C37004)
收稿日期 2017/9/1
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备注黄超群,硕士研究生,主要从事食品中农药残留检测,hcq@ziq.gov.cn
引用该论文: HUANG Chaoqun,HUANG Xue,WU Juan,CHEN Li,JI Yaojie. LC-MS/MS Determination of Residual Amounts of 5 Neonicotinoid Pesticides in Tea with Dispersive Solid Phase Extraction Using Multiwalled Carbon Nanotubes as Adsorbent[J]. Physical Testing and Chemical Analysis part B:Chemical Analysis, 2018, 54(5): 584~590
黄超群,黄雪,吴娟,陈丽,季垚杰. 多壁碳纳米管分散固相萃取-液相色谱-串联质谱法测定茶叶中5种烟碱类农药的残留量[J]. 理化检验-化学分册, 2018, 54(5): 584~590
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参考文献
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【2】张梅凤,范金勇,张宏伟,等.新烟碱类杀虫剂的研究进展[J].世界农药, 2009,31(1):22-25.
【3】GB 2763-2016食品安全国家标准食品中农药最大残留限量[S].
【4】Regulation (EC) No 396/2005 Maximum residue levels of pesticides in or on food and feed of plant and animal origin and amending council directive 91/414/EEC text with EEA relevance[S].
【5】European Commission. The rapid alert system for food and feed[EB/OL].[2017-08-30] . http://ec.europa.eu/food/safety/rasff/index_en.htm.
【6】GB/T 23379-2009水果、蔬菜及茶叶中吡虫啉残留的测定高效液相色谱法[S].
【7】NY/T 1724-2009茶叶中吡虫啉残留量的测定高效液相色谱法[S].
【8】GB 23200.13-2016食品安全国家标准茶叶中448种农药及相关化学品残留量的测定液相色谱-质谱法[S].
【9】SN/T 2561-2010进出口食品中吡啶类农药残留量的测定液相色谱-质谱/质谱法[S].
【10】李慧思,黄超群,蒋沁婷,等.在线净化-液相色谱-串联质谱法测定茶叶中5种烟碱类农药残留[J].色谱, 2016,34(3):263-269.
【11】赵海香,孙艳红,丁明玉,等.多壁碳纳米管固相萃取净化-高效液相色谱法测定猪肉和鸡肉中的磺胺多残留[J].色谱, 2014,32(3):294-298.
【12】HOU X L, WU Y L, YANG T, et al. Multi-walled carbon nanotubes-dispersive solid-phase extraction combined with liquid chromatography-tandem mass spectrometry for the analysis of 18 sulfonamides in pork[J]. Journal of Chromatography B, 2013,929:107-115.
【13】WU Y L, CHEN R X, XUE Y, et al. Simultaneous determination of amantadine, rimantadine and memantine in chicken muscle using multi-walled carbon nanotubes as a reversed-dispersive solid phase extraction sorbent[J]. Journal of Chromatography B, 2014,965:197-205.
【14】荣杰峰,韦航,李亦军,等.羟基化多壁碳纳米管分散固相萃取-气相色谱-质谱法测定茶叶中21种有机磷农药[J].色谱, 2016,34(2):194-201.
【15】HAN Y T, 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 a reversed-dispersive solid phase extraction materials[J]. Journal of Chromatography B, 2015,1005:56-64.
【16】HAN Y T, SONG L, ZOU N, et al. Multi-residue determination of 171 pesticides in cowpea using modified QuEChERS method with multi-walled carbon nanotubes as a reversed-dispersive solid-phase extraction materials[J]. Journal of Chromatography B, 2016,1031:99-108.
【17】DONG M F, SI W S, JIANG K Q, et al. Multi-walled carbon nanotubes as solid-phase extraction sorbents for simultaneous determination of type A trichothecenes in maize, wheat and rice by ultra-high performance liquid chromatography-tandem mass spectrometry[J]. Journal of Chromatography A, 2015,1423:177-182.
【18】LⅡGAND J, KRUVE A, LEITO I, et al. Effect of mobile phase on electrospray ionization efficiency[J]. Journal of the American Society for Mass Spectrometry, 2014,25:1853-1861.
【19】SANTE/11945/2015 Guidance document on analytical quality control and method validation procedures for pesticides residues analysis in food and feed[S].
【20】粟有志,李芳,于晶晶,等.QuEChERS-高效液相色谱-串联质谱法测定植物源食品中氯啶菌酯和丙炔恶草酮残留[J].色谱, 2016,34(6):577-582.
【21】MATUSZEWSKI B K, CONSTANZER M L, CHAVEA-ENG C M. Strategies for the assessment of matrix effect in quantitative bioanalytical methods based on HPLC-MS/MS[J]. Analytical Chemistry, 2003,75(13):3019-3030.
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