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. doi: 10.16438/j.0513-4870.2019-0531
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. doi: 10.16438/j.0513-4870.2019-0531
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 spectrometryJ. Acta Pharmaceutica Sinica, 2020,55(1): 113-122. doi: 10.16438/j.0513-4870.2019-0531
Citation: 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 spectrometryJ. Acta Pharmaceutica Sinica, 2020,55(1): 113-122. doi: 10.16438/j.0513-4870.2019-0531

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

  • 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。

     

    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.

     

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