实时直接分析-高分辨质谱法快速筛查乳粉中抗生素残留  

Rapid Screening of Antibiotic Residues in Milk Powder Using Direct Analysis in Real Time High Resolution Mass Spectrometry

作　　者：杨帆 张璐琪 张鸿伟 纪仁春 张晓梅 许辉 王凤美 王妍婷 宫小明 徐杰[1] YANG Fan;ZHANG Lu-qi;ZHANG Hong-wei;JI Ren-chun;ZHANG Xiao-mei;XU Hui;WANG Feng-mei;WANG Yan-ting;GONG Xiao-ming;XU Jie(College of Food Science and Engineering,Ocean University of China,Qingdao 266003,China;Technology Center of Qingdao Customs District,Qingdao 266002,China;Technology Center of Xishuangbanna Customs District,Jinghong 666100,China;Technology Center of Weifang Customs District,Weifang 261041,China)

机构地区：[1]中国海洋大学食品科学与工程学院,山东青岛266003 [2]青岛海关技术中心,山东青岛266002 [3]西双版纳海关综合技术中心,云南景洪666100 [4]潍坊海关技术中心,山东潍坊261041

出　　处：《质谱学报》2021年第6期1014-1024,共11页Journal of Chinese Mass Spectrometry Society

基　　金：国家重点研发计划专项(2018YFC0311206);青岛市民生科技计划项目(18-6-1-107-nsh);青岛海关科技计划项目(QK201916);海关总署科技项目(2020HK201)。

摘　　要：建立了实时直接分析-高分辨质谱(DART-Q-Orbitrap HRMS)法快速检测乳粉中抗生素残留。通过优化DART载气类型、离子化温度、进样速度等条件,采用QuickStrip(QS)样品卡模块,以氦气作为载气,离子化温度400℃,进样速度1 mm/s,使用四极杆-离子回旋轨道阱高分辨质谱仪(Q-Orbitrap)在正离子模式下直接进样分析。结果表明,该方法能够完成16种常见磺胺类、喹诺酮类和大环内酯类抗生素的筛查检测,筛查限浓度水平为100μg/kg,回收率在72.5%~106.7%之间,假阴性率≤5%,且通过实际样品检测验证了此筛查方法的可行性。该方法前处理简单、分析速度快、结果可靠,能够满足乳粉中抗生素残留快速筛查分析的要求。Antibiotic residues in milk powder are public focusing concerns relevant to food safety.Long-term exposure to antibiotic residues will lead to drug-resistant strains in human body,reduce body's immunity,and bring health hazards to consumers.Sulfonamides,(fluoro)quinolones and macrolides are high-frequency detecting antibiotic residues in matrix of milk powder.Rapid screening analysis of these residues and simultaneous confirmation with high confidence are valuable in practical scenarios of investigation testing,special monitoring program and so on.The direct analysis in real time(DART)ion source is an emerging technology of ambient pressure desorption ionization,it can directly complete the analysis of sample ionization and injection at the ambient pressure and open experimental environment,without changing the properties of the analyte itself.It became possible to analyze samples directly with minimal sample preparation steps or even without any sample pretreatment procedure with DART ion source.A hybrid high resolution mass spectrotmety,quadrupole-orbitrap high resolution mass spectrometry(Q-Orbitrap HRMS)is a powerful tool in veterinary drug residue analysis with superior specificity,accuracy and sensitivity.In present study,DART ion source was hyphenated to Q-Orbitrap HRMS to perform rapid screening analysis and simultaneously unambiguous identification of the above-mentioned antibiotic residues in milk powder.Sample was diluted in water and fast purified by filtering solid phase extraction column and then the filtrate was subjected to DART-Q-Orbitrap HRMS analysis.Several key parameters of the DART ion source,such as ionization type and temperature,as well as injection speed of DART ion source were optimized to enhance the performance of the method.Then,a QuickStrip(QS)Module was selected with the helium as carrier gas and ionization temperature as well as injection speed were set to 400℃and 1 mm/s,respectively.The DART ion source with optimized settings coupled to Q-Orbitrap HRMS was finally applied to sc

关 键 词：乳粉 抗生素残留 实时直接分析(DART) 高分辨质谱 筛查 

分 类 号：O657.63[理学—分析化学]