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  

Qualitative screening of 169 veterinary drug residues in bear bile powder by QuEChERS-ultra high performance liquid chromatography-tandem mass spectrometry

作　　者：孙健[1] 胡青[1] 诸艳蓉[1] 张甦[1] 于泓[1] 冯睿[1] 张静娴[1] 毛秀红[1] 季申[1] 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)

机构地区：[1]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

出　　处：《药学学报》2020年第1期113-122,共10页Acta Pharmaceutica Sinica

基　　金：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)

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 000μg·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。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 Na2 EDTA-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.

关 键 词：QUECHERS 超高效液相色谱串联质谱 兽药 熊胆粉 定性筛查 

分 类 号：R917[医药卫生—药物分析学]