Simultaneous Screening and Analysis of 153 Veterinary Drug Residues in Raw Milk by One-step QuEChERS Combined with Liquid Chromatography Quadrupole Electrostatic Field Orbital Trap High Resolution Mass Spectrometry

TONG Kai-xuan; CHANG Qiao-ying; XIE Yu-jie; WU Xing-qiang; FAN Chun-lin; CHEN Hui

doi:10.19969/j.fxcsxb.23062802

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Simultaneous Screening and Analysis of 153 Veterinary Drug Residues in Raw Milk by One-step QuEChERS Combined with Liquid Chromatography Quadrupole Electrostatic Field Orbital Trap High Resolution Mass Spectrometry

Scientific Papers | 更新时间：2023-10-18

- Simultaneous Screening and Analysis of 153 Veterinary Drug Residues in Raw Milk by One-step QuEChERS Combined with Liquid Chromatography Quadrupole Electrostatic Field Orbital Trap High Resolution Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 10, Pages: 1279-1290(2023)
- 作者机构：
  
  中国检验检疫科学研究院，国家市场监管重点实验室（食品质量与安全），北京 100176
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23062802
  CLC：
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仝凯旋,常巧英,谢瑜杰等.一步式QuEChERS结合液相色谱-四极杆/静电场轨道阱高分辨质谱同时筛查与分析生牛乳中153种兽药残留[J].分析测试学报,2023,42(10):1279-1290.

TONG Kai-xuan,CHANG Qiao-ying,XIE Yu-jie,et al.Simultaneous Screening and Analysis of 153 Veterinary Drug Residues in Raw Milk by One-step QuEChERS Combined with Liquid Chromatography Quadrupole Electrostatic Field Orbital Trap High Resolution Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1279-1290.
仝凯旋,常巧英,谢瑜杰等.一步式QuEChERS结合液相色谱-四极杆/静电场轨道阱高分辨质谱同时筛查与分析生牛乳中153种兽药残留[J].分析测试学报,2023,42(10):1279-1290. DOI： 10.19969/j.fxcsxb.23062802.

TONG Kai-xuan,CHANG Qiao-ying,XIE Yu-jie,et al.Simultaneous Screening and Analysis of 153 Veterinary Drug Residues in Raw Milk by One-step QuEChERS Combined with Liquid Chromatography Quadrupole Electrostatic Field Orbital Trap High Resolution Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1279-1290. DOI： 10.19969/j.fxcsxb.23062802.

摘要

该文建立了液相色谱-四极杆/静电场轨道阱高分辨质谱（LC-Q Orbitrap HRMS）同时筛查与定量生牛乳基质中15类153种兽药的方法。生牛乳样品加入6 mL Na,2,EDTA-McIlvaine缓冲液，经10 mL 1%（体积分数）乙酸酸化乙腈提取，30 mg PSA和90 mg C,18,净化后，以0.1%甲酸水溶液和乙腈为流动相，Agilent Eclipse plus C,18,柱分离，分别在Full MS/dd-MS,2,正离子和负离子模式下进行检测。在最优条件下对方法学参数进行验证，各类兽药在相应浓度范围内线性关系良好，线性系数（,r,2,）在0.99以上，所有兽药的筛查限（SDL）为0.1~20 μg/kg，定量下限（LOQ）为0.1~20 μg/kg，在1倍LOQ、2倍LOQ和10倍LOQ 3个加标水平下进行回收率实验，目标兽药的回收率为70%~120%，且相对标准偏差（RSD）≤20%的占比分别为92.8%、94.1%和94.8%。该方法样品处理简单、耗时短且灵敏度高，适用于生牛乳中多类兽药的快速筛查与定量。

Abstract

In this paper，a screening and quantitative method for 15 kinds of 153 veterinary drugs in raw milk matrix was established by one-step QuEChERS combined with liquid chromatography quadrupole electrostatic field orbital trap high resolution mass spectrometry（LC-Q Orbitrap HRMS）. Raw milk samples were added with 6 mL of Na,2,EDTA-McIlvine buffer，extracted with acetonitrile acidified with 1%（by volume） acetic acid，purified with 30 mg PSA and 90 mg C,18,，separated on an Agilent Eclipse plus C,18, column using 0.1% formic acid aqueous solution and acetonitrile as mobile phase，and detected in full MS/dd-MS,2, positive ion scanning mode. All kinds of veterinary drugs had good linearities in the corresponding concentration ranges，and the correlation coefficient（,r,2,） were above 0.99. The limits of screening（SDL） of all veterinary drugs were in the range of 0.1-20 μg/kg，and the limits of quantitation（LOQ） were in the range of 0.1-20 μg/kg. The recoveries were verified at three spiked levels of 1-，2- and 10- times LOQ（,n,=6）. The recoveries of target veterinary drugs at three spiked levels ranged from 70% to 120%，and the relative standard deviations（RSDs）≤20% accounted for 92.8%，94.1% and 94.8%，respectively. This method has the advantages of simple sample processing，short time consumption，and high sensitivity，making it suitable for rapid screening and quantification of multiple types of veterinary drugs in raw milk.

关键词

生牛乳液相色谱-四极杆/静电场轨道阱高分辨质谱（LC-Q Orbitrap HRMS）兽药残留

Keywords

raw milkliquid chromatography quadrupole electrostatic field orbital trap high resolution mass spectrometry（LC-Q Orbitrap HRMS）veterinary drugs

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