摘要
目的建立液相色谱-串联质谱法(liquid chromatography-tandem mass spectrometry,LC-MS/MS)测定猪油与猪肉中阿托品、普鲁卡因、东莨菪碱、山莨菪碱和利多卡因等5种药物的分析方法。方法优化前处理条件及仪器参数,使用HLB Pro固相萃取小柱净化,1 m L 30%乙腈和1 m L纯乙腈洗脱。在5 k V毛细管高压,540℃13 L/min去溶剂气,2 L/min雾化气,1.2 L/min反吹气,多反应监测模式等条件下测定猪油与猪肉中5种兽药残留。结果5种药物在0.1~10.0 ng/m L质量浓度范围内相关系数(r^(2))大于等于0.9981,定量限在0.013~0.142μg/kg,回收率在84.72%~106.24%,精密度在0.45%~7.32%(n=6),测试的猪油与猪肉样品中未检出药物残留。结论本研究基于LC-MS/MS和HLB pro固相萃取柱建立的检测方法,为猪肉和猪油中5种兽药残留的高效筛查提供了经济可靠的解决方案。
Objective To establish a method for the determination of 5 kinds of drugs(atropine,procaine,scopolamine,anisodamine and lidocaine)in lard and pork by liquid chromatography-tandem mass spectrometry(LC-MS/MS).Methods The pretreatment conditions and instrument parameters were optimized.HLB Pro solid-phase extraction cartridges were used for purification,with 1 mL of 30%acetonitrile and 1 mL of pure acetonitrile for elution.The residues of the 5 kinds of veterinary drugs in lard and pork were determined under the following conditions:5 kV capillary voltage,540°C desolvation gas temperature at 13 L/min,2 L/min nebulizer gas flow,1.2 L/min cone gas flow,and multiple reaction monitoring mode.Results The calibration curves of the 5 kinds of drugs showed good linearity in the mass concentration range of 0.1-10.0 ng/mL,with correlation coefficient(r^(2))>0.9950.The limits of quantitation ranged from 0.013 to 0.142μg/kg.Recoveries were between 84.72%and 106.24%,and precision(n=6)ranged from 0.45%to 7.32%.No target drug residues were detected in the tested pork and lard samples.Conclusion This study establishes a detection method based on a domestically produced LC-MS/MS system and HLB Pro solid-phase extraction columns,providing a cost-effective and reliable solution for the efficient screening of the 5 kinds of veterinary drug residues in pork and lard.
作者
刘磊
杨继伟
周颖
李剑
童文烽
徐巧
LIU Lei;YANG Ji-Wei;ZHOU Ying;LI Jian;TONG Wen-Feng;XU Qiao(Hangzhou Puyu Technology Development Co.,Ltd.,Hangzhou 311305,China;Zhejiang Grain and Oil Trade Co.,Ltd,Hangzhou 311305,China)
出处
《食品安全质量检测学报》
2025年第15期65-72,共8页
Journal of Food Safety and Quality
关键词
液相色谱-串联质谱法
猪油
猪肉
药物残留
固相萃取法
liquid chromatography-tandem mass spectrometry
pork
lard
drug residues
solid-phase extraction
