乳业科学与技术2024,Vol.47Issue(2) :24-29.DOI:10.7506/rykxyjs1671-5187-20240409-018

QuEChERS-超高效液相色谱-四极杆/静电场轨道阱质谱法测定牛羊乳及其乳粉中21种兽药

Determination of 21 Veterinary Drugs in Cow and Goat Milk and Milk Powder by QuEChERS Combined with Ultra Performance Liquid Chromatography-Quadrupole/Orbitrap Mass Spectrometry

张申平 秦宇 顾颖娟
乳业科学与技术2024,Vol.47Issue(2) :24-29.DOI:10.7506/rykxyjs1671-5187-20240409-018

QuEChERS-超高效液相色谱-四极杆/静电场轨道阱质谱法测定牛羊乳及其乳粉中21种兽药

Determination of 21 Veterinary Drugs in Cow and Goat Milk and Milk Powder by QuEChERS Combined with Ultra Performance Liquid Chromatography-Quadrupole/Orbitrap Mass Spectrometry

张申平 1秦宇 2顾颖娟1
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作者信息

  • 1. 上海市质量监督检验技术研究院/国家市场监管重点实验室(乳及乳制品检测与监控技术),上海 200233
  • 2. 上海市质量监督检验技术研究院/国家市场监管重点实验室(乳及乳制品检测与监控技术),上海 200233;华东理工大学生物工程学院,上海 200237
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摘要

采用QuEChERS方法处理样品,使用超高效液相色谱-四极杆/静电场轨道阱质谱(ultra performance liquid chromatography-quadrupole/orbitrap mass spectrometry,UPLC-Q/Orbitrap MS)进行测定,建立牛羊乳及其乳粉中21种兽药的分析方法.通过优化色谱条件、质谱参数和前处理条件,确定最佳测试方法.样品经乙腈盐析超声提取后,采用N-丙基乙二胺和C18净化,经Accucore RP-MS色谱柱(100 mm×2.1 mm,2.7 μm)分离,UPLC-Q/Orbitrap MS测定.结果表明:21种兽药在各自线性范围内具有良好的线性关系,相关系数(r2)均大于0.99;方法定量限为0.5 μg/kg;在0.5、2.0、10.0 μg/kg加标水平下的平均回收率为67.2%~110.2%,相对标准偏差为3.6%~17.4%(n=6).该方法简便、灵敏,适用于牛羊乳及其乳粉中21种兽药的同步检测.

Abstract

A method for the determination of 21 veterinary drugs in cow and goat milk and milk powder was established by the QuEChERS(quick,easy,cheap,effective,rugged,safe)sample pretreatment method combined with ultra performance liquid chromatography-quadrupole/orbitrap mass spectrometry(UPLC-Q/Orbitrap MS).Chromatographic conditions,mass spectrometric parameters and pretreatment conditions were optimized.Samples were extracted with acetonitrile in the presence of anhydrous sodium sulfate,purified using a mixture of primary secondary amine(PSA)and C18,separated on an Accucore RP-MS column(100 mm × 2.1 mm,2.7 μm),and detected by UPLC-Q/Orbitrap MS.Good linearity was observed for all the analytes in the investigated concentration ranges with correlation coefficients(r2)of greater than 0.99.The limit of quantification(LOQ)of the proposed method was 0.5 μg/kg.The average recoveries at spiked concentration levels of 0.5,2.0 and 10.0 μg/kg were 67.2%-110.2%with relative standard deviations(RSDs)of 3.6%-17.4%(n=6).The method is simple and sensitive,and suitable for simultaneous detection of the 21 veterinary drugs in cow and goat milk and milk powder.

关键词

QuEChERS/静电场轨道阱质谱/抗虫药/消炎药/糖皮质激素

Key words

QuEChERS/electrostatic field orbitrap mass spectrometry/antiparasitics/antiphlogistics/glucocorticoids

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基金项目

上海市质量监督检验技术研究院项目(KY-2022-2-SP)

出版年

2024
乳业科学与技术
上海奶业行业协会 光明乳业股分有限公司技术中心 上海市奶牛研究所 上海乳品培训研究中心

乳业科学与技术

CSTPCD
影响因子:0.619
ISSN:1671-5187
参考文献量22
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