用替代对照品法和质谱数据库快速筛查保健品或中成药中添加镇静安神类药品

发布时间：2018-02-26 23:36

  本文关键词： 中成药 保健品 镇静安神类化学药品 替代对照品法 高效液相色谱-质谱/质谱联用 二级质谱库　出处：《药物分析杂志》2015年01期 　论文类型：期刊论文

【摘要】：目的:建立中成药及保健品中添加镇静安神类化学药品的HPLC-DAD及HPLC-MS/MS分析方法,建立HPLC-DAD数据库及二级质谱库,并应用分析。方法:HPLC-DAD法采用Agilent ZORBAX Eclipse Plus C8(4.6 mm×150 mm,5μm)色谱柱,0.02 mmol·L-1磷酸二氢钾-甲醇(95∶5)为流动相,流速1.0 m L·min-1;HPLC-MS/MS法采用Shim-Pack VP-ODS(150 mm×2.0 mm,5μm)色谱柱,0.1%甲酸-乙腈为流动相,梯度洗脱,流速0.3 m L·min-1,质谱检测器以正离子和MRM方式进行检测。样品以甲醇为溶剂,超声提取。结果:HPLC-DAD法采用有效相对保留时间和紫外光谱相似度双指标进行定性准确可靠,相对校正因子法回收率98%~105%。优化HPLC-MS/MS条件,确定了定性离子及建立质谱库的最佳质谱条件。结论:该法快速准确,适用于中成药及保健品中非法添加镇静安神类化学药的质量监控,为替代对照品法及二级质谱库在此类研究中提供依据。
[Abstract]:Objective: to establish a HPLC-DAD and HPLC-MS/MS analysis method for the addition of sedative and tranquilizing chemicals in Chinese patent medicine and health care products, and to establish a HPLC-DAD database and a secondary mass spectrometry library. The mobile phase was 0.02 mmol 路L ~ (-1) potassium dihydrogen phosphate and methanol 95: 5). The flow rate was 1.0 mL 路min -1 HPLC-MS / MS. The mobile phase was Shim-Pack VP-ODS(150 mm 脳 2.0 mm ~ (5 渭 m). The mobile phase consisted of 0.1% formic acid-acetonitrile. The flow rate was 0.3 mL 路min-1, and the mass spectrometer was detected by positive ion and MRM. The sample was extracted with methanol and ultrasonic. Results the effective relative retention time and UV spectral similarity were determined by using effective relative retention time and UV spectrum similarity. The recovery rate of relative correction factor method was 98 ~ 105. The HPLC-MS/MS conditions were optimized, and the optimum mass spectrometry conditions for qualitative ion and mass spectrometry library were determined. Conclusion: this method is rapid and accurate, and is suitable for the quality control of the illegal addition of sedative and tranquilizing chemicals in Chinese patent medicine and health care products. It provides the basis for replacing the reference substance method and the secondary mass spectrometry library in this kind of research.
【作者单位】： 东营市食品药品检验中心;北京中医药大学;
【基金】：化学新药质量标准研究与评价技术平台(2011ZX09303-001)
【分类号】：R927;O657.63
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本文编号：1540207