猪肉中16种β-内酰胺类抗生素UPLC-Q-Orbitrap检测方法研究  

Screening and quantification of 16 β-lactam antibiotics in pork by UPLC-Q-Orbitrap

作　　者：潘晓东[1] 黄百芬[1] 张京顺[1] 蔡增轩[1] PAN Xiao-dong;HUANG Bai-fen;ZHANG Jing-shun;CAI Zeng-xuan(Zhejiang Provincial Center for Disease Control and Prevention,Hangzhou,Zhejiang 310051,China)

机构地区：[1]浙江省疾病预防控制中心

出　　处：《预防医学》2019年第11期1100-1104,共5页CHINA PREVENTIVE MEDICINE JOURNAL

基　　金：浙江省分析测试科技计划项目(2018C37018);浙江省医药卫生科技计划项目(2019316301);省部共建项目(WKJ-zj-1917)

摘　　要：目的采用高效液相色谱-四极杆/静电场轨道阱质谱法(UPLC-Q-Orbitrap)快速筛查并定量分析猪肉中16种β-内酰胺类抗生素.方法样品采用乙腈提取溶剂进行超声提取,离心取上清液,经HLB固相萃取柱净化,采用Waters HSS T3色谱柱(100 mm×2.1 mm,1.8μm)分离,梯度洗脱.质谱采用正离子扫描,Targeted SIM/dd-MS2监测模式,在10 min内完成对样品中分析物的分离和一级、二级质谱扫描.比较样品与对照品的色谱保留时间、一级质谱和二级质谱,确定样品中是否含有被测抗生素,并对阳性样品进行定量分析.结果16种β-内酰胺类抗生素在5~400 ng/mL范围内具有良好的线性关系(相关系数均>0.99),检出限为0.08~0.41μg/kg,回收率为85.5%~116.7%,相对标准偏差(RSD)为3.6%~12.8%.采用本方法对20份市售猪肉样品检测,其中1份检出青霉素G 28μg/kg,氨苄西林18.5μg/kg.结论UPLC-Q-Orbitrap法分辨率高,能减少样品基质干扰,提高定性和定量检测结果的准确性;且检测过程简便,分析时间短,检测效率高,适合对猪肉中β-内酰胺类抗生素进行筛查和定量检测.Objective To screen and quantify 16 kinds of β-lactam antibiotics in pork by high performance liquid chromatography-quadrupole/electrostatic field orbit trap mass spectrometry(UPLC-Q-Orbitrap). Methods The pork samples were extracted by ultrasound with acetonitrile,then the supernatant was centrifuged and purified by HLB solid phase extraction column. The analytes were separated by Waters HSS T3 column(100 mm ×2.1 mm,1.8 μm) with gradient elution. Mass spectrometry adopted positive ion scanning and targeted SIM/dd-MS2 monitoring mode to complete the separation of analytes in samples and mass spectrometry analysis within 10 minutes. The chromatographic retention time and fragments in mass spectrometry were compared with prepared standards to determine whether the samples contained the antibiotics tested, then the positive samples were quantified. Results The 16 kinds of β-lactam antibiotics had good linear relationship in the range of 5-400 ng/m L(all the correlation coefficients >0.99). The detection limits ranged from 0.08 μg/kg to 0.41 μg/kg,recovery rate ranged from85.5% to 116.7%,and relative standard deviation(RSD) ranged from 3.6% to 12.8%. One of twenty pork samples detected was found penicillin G(28 μg/kg) and ampicillin(18.5 μg/kg). Conclusion UPLC-Q-Orbitrap has high resolution and can reduce matrix interference to improve the accuracy. This method is simple,fast and efficient,thus can be used to screen and quantify β-lactam antibiotics in pork.

关 键 词：高效液相色谱 四极杆/静电场轨道阱质谱 猪肉 Β-内酰胺类抗生素 定量分析 

分 类 号：R155.5[医药卫生—营养与食品卫生学]