摘要
目的:本文建立金鸡颗粒中两面针鉴别方法,同时确认了金鸡颗粒掺伪特征成分毛两面针素,建立相应的分析方法。方法:采用薄层色谱法对两面针进行定性鉴别,对金鸡颗粒掺伪特征成分毛两面针素采用TLC初筛、HPLC验证、HPLC-MS/MS进行确证。在此基础上,采用高效液相色谱法对阳性样品中的毛两面针素进行含量测定。色谱条件:采用Hypersil DBS C18(250 mm×4.6 mm,5μm)色谱柱,以乙腈-0.1%磷酸溶液(21∶79)为流动相,流速0.8 mL/min,检测波长330 nm。结果:对21批金鸡颗粒进行了检测,并采用HPLC-MS/MS对可疑样品进行确认,其中3批次检出毛两面针素;毛两面针素进样在0.07332~2.444μg的范围内有良好的线性关系。3批次阳性样品中毛两面针素的含量范围为65.48~73.94μg/g。结论:本方法准确可靠,可作为金鸡颗粒中两面针掺伪的检测方法。
Objective:To establish the identification method of Toddalolactone in Jinji granules.Toddalolactone was identified as characteristic component when Jinji granules is adulterated and corresponding method was developed.Methods:TLC was used for qualitative identification of Zanthorulum nitidum,TLC,HPLC and HPLC-MS/MS were used for confirmation.Based on those results,HPLC method was developed for the qualification of toddalolactone in positive samples.An Hypersil BDS C18(250 mm×4.6 mm,5μm)column was adopted,the mixture of acetonitrile-0.1%phosphoric acid solution(21∶79)was used as the mobile phase,the flow rate was 0.8 mL/min,and the detection wavelength was set at 330 nm.Results:21 batches of Jinji granules were tested,the suspected samples were confirmed by HPLC-MS/MS.Toddalolactone was detected from 3 batches of samples.The linear range of toddalolactone was 0.07332-2.444μg.The content of toddalolactone in three batches of positive samples ranged from 65.48 to 73.94μg/g.Conclusion:This method is accurate and reliable,and can be used as the detection method for toddalolactone in Jinji granules.
作者
胡亮
李瑞莲
王银红
HU Liang;LI Ruilian;WANG Yinhong(Hunan Institute for Drug Control,Hunan Pharmaceutical Excipients Testing and Inspection Center,Changsha 410001,China;Hunan Engineering&Technology Research Center for Pharmaceutical Quality Evaluation,Changsha 410001,China)
出处
《药品评价》
CAS
2020年第15期19-22,30,共5页
Drug Evaluation
基金
湖南省自然科学基金项目(2020JJ9012)。
