药学学报, 2020, 55(1): 113-122
引用本文:
孙健, 胡青, 诸艳蓉, 张甦, 于泓, 冯睿, 张静娴, 毛秀红, 季申. QuEChERS-超高效液相色谱串联质谱法定性筛查中药材熊胆粉中169种兽药残留[J]. 药学学报, 2020, 55(1): 113-122.
SUN Jian, HU Qing, ZHU Yan-rong, ZHANG Su, YU Hong, FENG Rui, ZHANG Jing-xian, MAO Xiu-hong, JI Shen. Qualitative screening of 169 veterinary drug residues in bear bile powder by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry[J]. Acta Pharmaceutica Sinica, 2020, 55(1): 113-122.

QuEChERS-超高效液相色谱串联质谱法定性筛查中药材熊胆粉中169种兽药残留
孙健, 胡青, 诸艳蓉, 张甦, 于泓, 冯睿, 张静娴, 毛秀红, 季申
上海市食品药品检验所, 国家药品监督管理局中药质量控制重点实验室, 上海 201203
摘要:
建立了QuEChERS-超高效液相色谱串联质谱法定性筛查中药材熊胆粉中多种兽药残留,包括β-受体激动剂与拮抗剂、抗生素(青霉素类、头孢菌素类、磺胺类、喹诺酮类、氯霉素类、四环素类、硝基咪唑类、大环内酯类、聚醚类等)、抗病毒药、驱虫药、甾体激素、非甾体抗炎药和镇静剂等169种兽药残留。样品经Na2EDTA-McIlvaine缓冲液和5%甲酸乙腈提取,经分散固相萃取法净化,以超高效液相色谱串联三重四极杆质谱法测定,通过离子丰度比定性判定。169种化合物检出限为1~1 000 μg·kg-1。本方法简便快速,已应用于实际样品的测定,并可扩展至其他类似药材基质的检测。
关键词:    QuEChERS      超高效液相色谱串联质谱      兽药      熊胆粉      定性筛查     
Qualitative screening of 169 veterinary drug residues in bear bile powder by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry
SUN Jian, HU Qing, ZHU Yan-rong, ZHANG Su, YU Hong, FENG Rui, ZHANG Jing-xian, MAO Xiu-hong, JI Shen
NMPA Key Laboratory for Quality Control of Traditional Chinese Medicine, Shanghai Institute for Food and Drug Control, Shanghai 201203, China
Abstract:
A QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry method was developed for qualitative screening of 169 veterinary drug residues in bear bile powder, including β-agonists and inhibitors, antibiotics (penicillins, β-lactams, sulfomamides, quinolones, chloramphenicals, tetracyclines, nitroimidazoles, macrolides, polyethers, etc.), antiviral drugs, anthelminitics, steroid hormones, nonsteroidal antiinflammatory drugs (NSAIDs) and sedatives. The samples were extracted by Na2EDTA-McIlvaine buffer solution and 5% fomic acid-acetonitrile solution, then purified by dispersive solid phase extraction. Detection of veterinary drug residues by ultra high performance liquid chromatography-triple quadrupole mass spectrometry was conducted and qualitative confirmed by ion ratios. The limits of detection of 169 veterinary drugs were 1-1 000 μg·kg-1. The method is simple and fast, which had been used for the analysis of actual samples, and can be extended to the detection of similar matrix.
Key words:    QuEChERS    ultra high performance liquid chromatography-tandem mass spectrometry    veterinary drug    bear bile powder    qualitative screening   
收稿日期: 2019-07-05
DOI: 10.16438/j.0513-4870.2019-0531
基金项目: 国家中药标准化项目(ZYBZH-C-SH-48);上海市科委技术平台项目(18DZ2292200);上海市科委技术标准专项(18DZ2200900);上海市科委课题(18395810300).
通讯作者: 季申,Tel:86-21-50798195,E-mail:jishen2013@163.com
Email: jishen2013@163.com
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