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

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,5 μm)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 mL·min^-1;HPLC-MS/MS法采用Shim-Pack VP-ODS(150 mm×2.0 mm, 5 μm)色谱柱,0.1%甲酸-乙腈为流动相,梯度洗脱,流速0.3 mL·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.

Objective: To establish an HPLC-DAD and HPLC-MS/MS method for detecting sedative hypnotic drugs illegally added in Chinese patent drugs and health products and to establish database and secondary mass spectral libraries for application and analysis. Methods: For the HPLC-DAD method, the column was Agilent ZORBAX Eclipse Plus C₈ (4.6 mm×150 mm,5 μm); the mobile phase was 0.02 mmol·L^-1 potassium dihydrogen phosphate solution-methanol (95:5); the flow rate was 1.0 mL·min^-1.For the HPLC-MS/MS method, the column was Shim-Pack VP-ODS (150 mm×2.0 mm, 5 μm); the mobile phase was 0.1% formic acid-acetonitrile by a gradient elution; the flow rate was 0.3 mmol·L^-1; the positive ion and the MRM system were used for mass spectrum detection; samples were prepared by ultrasonic extraction with methanol as the solvent. Results: Double indexes including effective relative retention time and ultraviolet spectrum similarity that were used in the qualitative analysis were reliable and accurate in the HPLC-DAD method.Recovery was 98%-105% by relative correction factor method.The qualitative ions and the best mass spectrometer conditions to establish mass spectral library were determined by optimizing HPLC-MS/MS conditions. Conclusion: The method was fast and accurate, and suitable for the quality monitoring of sedative hypnotic drugs illegally added in Chinese patent drugs and health products.The substitute reference substance and secondary mass spectral libraries provide a basis for studies in this field.