Rapid Screening of 69 Veterinary Drug Residues in Milk by Ultra-high Performance Liquid Chromatography-Quadrupole-Time-of-flight Mass Spectrometry

YAN Zu-hao; LI Xiao-wei; XIA Xi

doi:10.19969/j.fxcsxb.23070302

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Rapid Screening of 69 Veterinary Drug Residues in Milk by Ultra-high Performance Liquid Chromatography-Quadrupole-Time-of-flight Mass Spectrometry

Scientific Papers | 更新时间：2023-10-18

- Rapid Screening of 69 Veterinary Drug Residues in Milk by Ultra-high Performance Liquid Chromatography-Quadrupole-Time-of-flight Mass Spectrometry
- Journal of Instrumental Analysis Vol. 42, Issue 10, Pages: 1309-1318(2023)
- 作者机构：
  
  中国农业大学动物医学院，北京 100193
- 作者简介：
- 基金信息：
- DOI：10.19969/j.fxcsxb.23070302
  CLC：
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严祖浩,李晓薇,夏曦.牛奶中69种兽药残留的超高效液相色谱-四极杆-飞行时间质谱快速筛查[J].分析测试学报,2023,42(10):1309-1318.

YAN Zu-hao,LI Xiao-wei,XIA Xi.Rapid Screening of 69 Veterinary Drug Residues in Milk by Ultra-high Performance Liquid Chromatography-Quadrupole-Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1309-1318.
严祖浩,李晓薇,夏曦.牛奶中69种兽药残留的超高效液相色谱-四极杆-飞行时间质谱快速筛查[J].分析测试学报,2023,42(10):1309-1318. DOI： 10.19969/j.fxcsxb.23070302.

YAN Zu-hao,LI Xiao-wei,XIA Xi.Rapid Screening of 69 Veterinary Drug Residues in Milk by Ultra-high Performance Liquid Chromatography-Quadrupole-Time-of-flight Mass Spectrometry[J].Journal of Instrumental Analysis,2023,42(10):1309-1318. DOI： 10.19969/j.fxcsxb.23070302.

摘要

建立了超高效液相色谱-四极杆-飞行时间质谱快速筛查牛奶中,β,-受体激动剂类、磺胺类、喹诺酮类、四环素类4类共69种兽药残留量的分析方法。牛奶用含0.5%甲酸的乙腈溶液提取，乙腈饱和的正己烷净化除脂，使用ACQUITY UPLC BEH C,18,色谱柱分离，以0.1%甲酸和含0.1%甲酸的甲醇-乙腈（2∶8）为流动相梯度洗脱，10 min内可实现69种兽药的良好分离，在电喷雾离子源（ESI）正离子模式下运用全扫描和数据依赖采集（DDA）方式进行测定。牛奶中69种兽药的定量下限（LOQ）为10 μg·kg,-1,；在10、50、100 μg·kg,-1,下的平均加标回收率为59.0%～120%，相对标准偏差（RSD）为0.80%～13%。该方法操作简单，检测效率高，可用于牛奶中69种兽药的快速筛查。

Abstract

An ultra-high performance liquid chromatography-quadrupole-time-of-flight mass spectrometry method was developed for rapid screening of 69 veterinary drugs belonging to four classes（,β,-agonists，sulfonamides，quinolones and tetracyclines） in milk. The extraction was performed using acetonitrile solution containing 0.5% formic acid，and the purification was carried out by liquid-liquid extraction using ,n,-hexane for defatting. An ACQUITY UPLC BEH C,18, column was used for chromatographic separation，and gradient elution was performed using 0.1% formic acid and methanol-acetonitrile（2∶8） containing 0.1% formic acid as the mobile phases. The electrospray ionization was used in positive ion mode for full scan and data-dependent acquisition mode（DDA） detection. Efficient separation of 69 veterinary drugs can be achieved within 10 min. The limits of quantification（LOQs） of 69 veterinary drugs in milk was 10 μg·kg,-1,. The average recoveries was 59.0%-120% with relative standard deviations（RSDs） of 0.80%-13% at three spiked levels（10，50 and 100 μg·kg,-1,）. This method is simple and efficient，and can be used for the rapid screening of 69 veterinary drugs in milk.

关键词

牛奶超高效液相色谱飞行时间质谱兽药残留快速筛查

Keywords

milkultra-high performance liquid chromatographytime-of-flight mass spectrometryveterinary drug residuesrapid screening

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