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液相色谱-飞行时间质谱法快速筛查生乳中29 种兽药残留的研究
引用本文:霍路曼,李艺,郑百芹,李明阳,张淼怡,郝立武,张书宏.液相色谱-飞行时间质谱法快速筛查生乳中29 种兽药残留的研究[J].中国乳业,2021,0(12):100-104.
作者姓名:霍路曼  李艺  郑百芹  李明阳  张淼怡  郝立武  张书宏
作者单位:河北省唐山市食品药品综合检验检测中心; 河北省农产品质量安全检测工程技术研究中心,河北唐山 063000
基金项目:河北省二期现代农业产业技术体系创新团队建设项目(HBCT2018120207); 河北省重点研发计划项目(19227516D)
摘    要:本文研究了用液相色谱串联飞行时间质谱建立生乳中29 种兽药残留的快速检测方法。生乳样品采用0.2%甲酸乙腈溶液提取上清液,采用Dikma ProElut QuECHERS净化管净化后测定。目标化合物通过Waters ACQUITY UPLC HSS T3色谱柱分离,以乙腈和1.0%甲酸水溶液为洗脱剂进行程序洗脱,正离子扫描模式检测。结果表明,通过对数据进行靶向分析,20.0 min内生乳中29 种兽药残留能够同时被检测出来,其中Mass Error在±2.0 mg/kg之内,Library Score得分均在90 分以上,准确性高,操作简便。

关 键 词:液相色谱-飞行时间质谱  生乳  兽药残留  测定  

Rapid Screening of 29 Veterinary Drug Residues in Raw Milk by Liquid Chromatography Coupled with Quadrupole-Time of Flight Mass Spectrometry
HUO Luman,LI Yi,ZHENG Baiqin,LI Mingyang,ZHANG Miaoyi,HAO Liwu,ZHANG Shuhong.Rapid Screening of 29 Veterinary Drug Residues in Raw Milk by Liquid Chromatography Coupled with Quadrupole-Time of Flight Mass Spectrometry[J].China Dairy,2021,0(12):100-104.
Authors:HUO Luman  LI Yi  ZHENG Baiqin  LI Mingyang  ZHANG Miaoyi  HAO Liwu  ZHANG Shuhong
Institution:Food and Drug Comprehensive Inspection and Testing Center of Tangshan,Hebei Province; Engineering Technology Research Center of Agricultural Product Quality and Safety Inspection of Hebei Province,Tangshan Hebei 063000
Abstract:The aim of this study was to establish a rapid method for 29 veterinary drug residues in raw milk by ultra liquid chromatography coupled with quadrupole-time of flight mass spectrometry(UPLC-Q-TOF-MS).The supernatant of raw milk was extracted from 0.2% formic acid acetonitrile solution and determined after purification by Dikma ProElut Quechers.The target compounds were separated by Waters ACQUITY UPLC HSS T3 column,and were eluted with acetonitrile and 1.0% formic acid aqueous solution,and detected in positive ion scanning mode. The results showed that through targeted analysis of the data,29 veterinary drug residues in raw milk could be detected at the same time within 20.0 minutes,of which the mass error was within ± 2 ppm and the library score was more than 90 points. The method has high accuracy and simple operation,and can meet the simultaneous and rapid determination of veterinary drug residues in raw milk sample 29.
Keywords:ultra liquid chromatography coupled with quadrupole-time of flight mass spectrometry  screening  raw milk  veterinary drug residues  detect  
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