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预防医学  2019, Vol. 31 Issue (11): 1100-1104    DOI: 10.19485/j.cnki.issn2096-5087.2019.11.005
  论著 本期目录 | 过刊浏览 | 高级检索 |
猪肉中16种β-内酰胺类抗生素UPLC-Q-Orbitrap检测方法研究
潘晓东,黄百芬,张京顺,蔡增轩
浙江省疾病预防控制中心,浙江 杭州 310051
Screening and quantification of 16 β-lactam antibiotics in pork by UPLC-Q-Orbitrap
PAN Xiao-dong,HUANG Bai-fen,ZHANG Jing-shun,CAI Zeng-xuan
Zhejiang Provincial Center for Disease Control and Prevention,Hangzhou,Zhejiang 310051,China
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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,1.8 μm)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0.08~0.41 μg/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 28 μg/kg,氨苄西林18.5 μg/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。
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潘晓东
黄百芬
张京顺
蔡增轩
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    
AbstractObjective 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/mL(all the correlation coefficients >0.99). The detection limits ranged from 0.08 μg/kg to 0.41 μg/kg,recovery rate ranged from 85.5% 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.
Key wordsHigh performance liquid chromatography    Quadrupole/electrostatic field orbit trap mass spectrometry    Pork    β-lactam antibiotics    Quantitative analysis
     出版日期: 2019-11-01
ZTFLH:  R155.5  
基金资助: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)
通信作者: 潘晓东,E-mail:xdpan@cdc.zj.cn   
作者简介: 潘晓东,博士,副研究员,主要从事理化检验工作
引用本文:   
潘晓东,黄百芬,张京顺,蔡增轩. 猪肉中16种β-内酰胺类抗生素UPLC-Q-Orbitrap检测方法研究[J]. 预防医学, 2019, 31(11): 1100-1104.
PAN Xiao-dong,HUANG Bai-fen,ZHANG Jing-shun,CAI Zeng-xuan. Screening and quantification of 16 β-lactam antibiotics in pork by UPLC-Q-Orbitrap. Preventive Medicine, 2019, 31(11): 1100-1104.
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http://www.zjyfyxzz.com/CN/10.19485/j.cnki.issn2096-5087.2019.11.005      或      http://www.zjyfyxzz.com/CN/Y2019/V31/I11/1100
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