液质联用法检测大活络丸和同仁大活络丸中贵毒药味和添加化合物

目的: 分别采用液质联用技术建立大活络丸和同仁大活络丸中贵毒药味检测方法和非法掺加镇痛、消炎类化学药品的专属性方法。 方法: 采用Agilent液相色谱-离子阱质谱联用仪,以Agilent ZORBAX SB-C₁₈(2.1 mm×150 mm,3.5 μm)色谱柱为固定相,以0.5%甲酸溶液-甲醇为流动相,梯度洗脱,流速为0.3 mL·min^-1,测定48种镇痛类化合物;以相同色谱柱,以水-乙腈为流动相,梯度洗脱,流速0.3 mL·min^-1,测定3味贵毒药味;质谱检测器采用ESI电离源,以正负离子切换自动扫描模式进行检测;供试品采用甲醇超声提取。通过与标准谱库中保留时间和多级质谱图的双重对比,分别对样品中非法掺加的化学药品和细辛、牛黄、血竭三味贵毒药味进行定性鉴别。 结果: 在229批供试品中,均检出麻黄碱,41批检出猪去氧胆酸,71批检出龙血素B。 结论: 该方法准确、快速、灵敏度高,为国内首次报道,为客观评价大活络丸和同仁大活络丸质量提供有力依据。

Objective: To establish separately specific methods by LC/MSⁿ for the identification of 3 valuable or toxic ingredients and 48 analgesic and anti-inflammatory chemical drugs added illegally into Dahuoluo pills and Tongren Dahuoluo pills . Methods: The detection of 48 compounds was performed by Agilent 1100 HPLC/MSD trap using Agilent ZORBAX SB-C₁₈(2.1 mm×150 mm,5 μm)column as stationary phase and 0.5%formic acid solution-methanol system as mobile phase .The gradient elution was done with as flow rate of 0.3 mL·min^-1.The detection of 3 valuable and toxic ingredients was performed by the same instrument and stationary phase,using water acetonitrile system in gradient elution as mobile phase.Positive and negative ionization switch autoscan mode was adopt using ESI source.Samples were extracted by Ultrasonic with methanol.Comparing with retention time and spectras of references in library set up by ourselves,the target compounds in sample are screened and identified. Results: There were ephedrine detected in 229 samples,hyodeoxycholic acid detected in 41 samples,and loureirin B detected in 71 samples. Conclusions: The methods were accurate,fast and sensitive.It was the first time in China to report the LC/MS method,which could evaluate the quality of samples objectively.