超高效液相色谱-四级杆-飞行时间串联质谱法检测中药及保健食品中21种非法添加的降脂类药物

Determination of 21 kinds of lipid-lowering drugs in herbal products and dietary supplements by ultra performance liquid chromatography/ quadrupole-time-of-flight mass spectrometry

中文关键词:  超高效液相色谱-四级杆-飞行时间串联质谱法  降脂类药物  中药  保健食品  非法添加

英文关键词:ultra performance liquid chromatography/quadrupole-time-of-flight mass spectrometry  lipid-lowering drugs  herbal products  dietary supplements  illegal additives

中文摘要:

      目的 建立超高效液相色谱-四级杆-飞行时间串联质谱仪(ultra performance liquid chromatography/ quadrupole-time-of-flight mass spectrometry, UPLC/Q-TOF-MS)快速检测中药及保健食品中的21种降脂类药物。方法 样品经甲醇超声提取后, 采用Agilent Poroshell 120 SB-C18色谱柱分离, 以0.1%甲酸水溶液和乙腈作为流动相进行梯度洗脱, 流速为0.4 mL/min; 质谱采用Q-TOF-MS作检测器, 采用电喷雾离子源(electronic spray ion, ESI)正负离子模式, 以保留时间、精确分子量和二级碎片比对进行定性分析。结果 21种降脂类药物的检出限为0.05~25 ng。对96批市售中成药及保健食品进行定性检测, 结果1批片剂中检出洛伐他丁, 其余均未检出。结论 本方法灵敏、准确、高效, 可适用常见降脂类药物的快速检测。

英文摘要:

      Objective To establish a method for determination of 21 kinds of lipid-lowering drugs in herbal products and dietary supplements by ultra performance liquid chromatography/quadrupole-time-of-flight mass spectrometry (UPLC/Q-TOF-MS). Methods The samples were processed by ultrasonic extraction with methanol, and separated by Agilent Poroshell 120 SB-C18 column with 0.1% formic acid and acetonitrile as mobile phase at the flow rate of 0.4 mL/min for gradient elution. Q-TOF-MS and electronic spray ion (ESI) both in positive and negative ionization mode were used in mass. Qualitative analysis was based on retention time, accurate mass, the elemental compositions and the product ions. Results The limits of detection (LOD) of 21 kinds of lipid-lowering drugs were 0.05~25 ng. Ninety-six batches of commercial herbal products and dietary supplements were detected, only 1 batch of tablet los simvastatin was detected, and the rest were not checked out. Conclusion The established method is sensitive, accurate and efficient, which is suitable for rapid determination of 21 kinds of lipid-lowering drugs in herbal products and dietary supplements.