Simultaneous Determination of Six Teicoplanins Residues in Fish Samples by High Performance Liquid Chromatography－Tandem Mass Spectrometry Coupled with QuEChERS Method

JIN Hui; ZHAO Cheng; ZHENG Guang-ming; WEI Lin-ting; SHI Xiao-na; LIN Jia-wei; LI Li-chun; SHAN Qi; MA Li-sha; YIN Yi

doi:10.19969/j.fxcsxb.21121403

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Simultaneous Determination of Six Teicoplanins Residues in Fish Samples by High Performance Liquid Chromatography－Tandem Mass Spectrometry Coupled with QuEChERS Method

Scientific Papers | 更新时间：2022-06-22

- Simultaneous Determination of Six Teicoplanins Residues in Fish Samples by High Performance Liquid Chromatography－Tandem Mass Spectrometry Coupled with QuEChERS Method
- Journal of Instrumental Analysis Vol. 41, Issue 6, Pages: 835-842(2022)
- 作者机构：
  
  1.上海海洋大学食品学院，上海 201306
  2.中国水产科学研究院珠江水产研究所/农业农村部水产品质量安全风险评估实验室（广州）/广东省水产动物免疫技术重点实验室，广东广州 510380
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.21121403
  CLC：
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金慧,赵城,郑光明等.QuEChERS技术结合高效液相色谱－串联质谱法测定鱼肉中6种替考拉宁残留量[J].分析测试学报,2022,41(06):835-842.

JIN Hui,ZHAO Cheng,ZHENG Guang-ming,et al.Simultaneous Determination of Six Teicoplanins Residues in Fish Samples by High Performance Liquid Chromatography－Tandem Mass Spectrometry Coupled with QuEChERS Method[J].Journal of Instrumental Analysis,2022,41(06):835-842.
金慧,赵城,郑光明等.QuEChERS技术结合高效液相色谱－串联质谱法测定鱼肉中6种替考拉宁残留量[J].分析测试学报,2022,41(06):835-842. DOI： 10.19969/j.fxcsxb.21121403.

JIN Hui,ZHAO Cheng,ZHENG Guang-ming,et al.Simultaneous Determination of Six Teicoplanins Residues in Fish Samples by High Performance Liquid Chromatography－Tandem Mass Spectrometry Coupled with QuEChERS Method[J].Journal of Instrumental Analysis,2022,41(06):835-842. DOI： 10.19969/j.fxcsxb.21121403.

摘要

采用QuEChERS前处理技术，建立了鱼肉中6种替考拉宁组分的高效液相色谱－串联质谱检测方法。搅碎均匀的鱼肉样品经乙腈-10%三氯乙酸（6∶4，体积比）提取，100 mg乙二胺-N-丙基硅烷（PSA）净化后，使用Agilent SB C,18,（2.1 mm × 100 mm，1.8 µm）色谱柱分离，以 0.1%甲酸乙腈和0.1%甲酸为流动相进行梯度洗脱，采用电喷雾电离正离子（ESI,+,），多反应监测模式（MRM）进行检测，内标法定量。考察了提取溶剂种类与体积、吸附剂种类与用量对目标化合物回收率的影响。评价了6种目标物在不同鱼肉基质中的基质效应。在优化条件下，6种替考拉宁组分在4 min内得到良好分离。目标物在各自浓度范围内线性良好，相关系数（,r,2,）均不小于0.998；在5.0、10.0、25.0 μg/kg 3个加标水平下，各组分的回收率为84.3%～93.3%，日内相对标准偏差和日间相对标准偏差（,n ,= 6）分别不大于7.0%和6.2%，方法的检出限和定量下限分别为0.5～2.0 μg/kg和2.0～5.0 μg/kg。采用该方法对采集的9种40个鱼肉样品进行检测，所有样品均未检出替考拉宁组分。该方法简单、灵敏、准确、可靠，可用于鱼肉中6种替考拉宁组分的定量分析。

Abstract

A high performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS） with QuEChERS pretreatment was developed for the simultaneous determination of six teicoplanins in fish samples．The six components in minced fish samples were extracted with acetonitrile－10% trichloroacetic acid（6∶4） mixed solution．Then the extracted supernatant was cleaned up with 100 mg of primary secondary amine（PSA）．Separation of the targets was performed on an Agilent SB C,18, chromatographic column（2.1 mm × 100 mm，1.8 µm） by gradient elution，using 0.1% formic acetonitrile and 0.1% formic as the mobile phase A and the mobile phase B，respectively．The six targets were detected in positive ion electrospray ionization mode（ESI,+,） under multiple reaction monitoring（MRM） mode，then quantified by the internal standard method with polymyxin sulfate B as the internal standard（IS）．Effects of different types and volumes of extraction solvent，different types and dosages of adsorbent on recoveries of six targets were investigated in detail．The matrix effects of six teicoplanins in different fish substrates were evaluated by the ratio of solvent standard curve and matrix-matched standard curve．Under the optimal conditions，six teicoplanins were well separated by HPLC－MS/MS within 4 min．Good linear relationships were obtained for six analytes in the concentration range of 1－100 μg/L，with their correlation coefficients（,r,2,） greater than 0.998．At three spiked levels of 5.0，10.0 and 25.0 μg/kg，the average recoveries for six analytes in different fish samples ranged from 84.3% to 93.3%，with intra-day relative standard deviations（intra－RSDs） and inter-day relative standard deviations（inter－RSDs） not more than 7.0% and 6.2%，respectively．The limits of detection（LODs） and limits of quantitation（LOQs） were in the range of 0.5－2.0 μg/kg and 2.0－5.0 μg/kg，respectively. The established method was applied to the detection of teicoplanins in various fish samples（forty fish samples that were divided into nine varieties，containing carp，crucian，grass carp，chub，silver carp，mandarin fish，tilapia，pseudosciaena crocea，and scophthalmus maximus） by random sampling principle，and no component of teicoplanin was detected in these actual samples．The developed method proved to be simple，sensitive，accurate and reliable，and was suitable for the simultaneous determination of six teicoplanins in fish samples.

关键词

替考拉宁QuEChERS技术高效液相色谱－串联质谱（HPLC－MS/MS）鱼肉

Keywords

teicoplaninsQuEChERShigh performance liquid chromatography－tandem mass spectrometry（HPLC－MS/MS）fish samples

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