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改良QuEChERS-超高效液相色谱-串联质谱法快速测定猪肉中12种利尿剂残留量

占昊 余晓峰 宣磊 孔维恒 刘雯 陈冉冉 蒙晓笛 周晓莹 吕亚宁 韩芳

肉类研究2025,Vol.39Issue(12):69-75,7.
肉类研究2025,Vol.39Issue(12):69-75,7.DOI:10.7506/rlyj1001-8123-20250223-054

改良QuEChERS-超高效液相色谱-串联质谱法快速测定猪肉中12种利尿剂残留量

Rapid Determination of 12 Diuretic Residues in Pork by Modified QuEChERS Combined with Ultra-high Performance Liquid Chromatography-Tandem Mass Spectrometry

占昊 1余晓峰 1宣磊 2孔维恒 3刘雯 1陈冉冉 1蒙晓笛 1周晓莹 1吕亚宁 1韩芳1

作者信息

  • 1. 合肥海关技术中心,安徽省食品安全监测与品控重点实验室,安徽 合肥 230022
  • 2. 安徽省体育科学技术研究所,国家体育总局运动训练监控与评定重点实验室,安徽 合肥 230011
  • 3. 中国海关科学技术研究中心,北京 100026
  • 折叠

摘要

Abstract

A method for the simultaneous determination of 12 diuretic residues in pork was developed using a modified QuEChERS approach and ultra-high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).After homogenization,the sample was extracted with acetonitrile and cleaned up with MgSO4,C18 and primary secondary amine.Separation was performed on an Eclipse Plus C18 column(100 mm×2.1 mm,1.8 μm)using a mobile phase consisting of 3 mmol/L ammonium formate-0.1%formic acid in water and acetonitrile.Detection was carried out using UPLC-MS/MS in the multiple reaction monitoring(MRM)mode.All analytes exhibited good linearity over the concentration range evaluated with correlation coefficients(R2)>0.99.The limits of quantitation(LOQ)were 2-5 μg/kg.The average recoveries at three spiked levels of LOQ,2 LOQ and 10 LOQ ranged from 85.8%to 112.0%,with relative standard deviations(RSDs)of 0.5%-5.1%.The proposed method is a simple yet efficient,sensitive and selective approach for the rapid detection of the 12 diuretics in pork.

关键词

QuEChERS/超高效液相色谱-串联质谱法/利尿剂/猪肉

Key words

QuEChERS/ultra-high performance liquid chromatography-tandem mass spectrometry/diuretics/pork

分类

化学化工

引用本文复制引用

占昊,余晓峰,宣磊,孔维恒,刘雯,陈冉冉,蒙晓笛,周晓莹,吕亚宁,韩芳..改良QuEChERS-超高效液相色谱-串联质谱法快速测定猪肉中12种利尿剂残留量[J].肉类研究,2025,39(12):69-75,7.

基金项目

"十四五"国家重点研发计划重点专项(2023YFF0611501) (2023YFF0611501)

国产质谱类设备海关验证评价技术和体系研究项目(2023HK141) (2023HK141)

肉类研究

OA北大核心

1001-8123

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