金鸡片中毛两面针素检测方法考察

Experimental Research on the Detection Methods for Toddalolactone in Jinji Tablets

目的:确认金鸡片中毛两面针素成分,建立相应的分析方法。方法:采用Hypersil DBS C_(18)(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^(-1),检测波长330 nm,采用液相色谱-质谱联用以及对照试剂对照的方法,对金鸡片中毛两面针素成分进行确证;通过薄层色谱和高效液相色谱法检测毛两面针素成分。结果:对58批金鸡片进行了检测,其中20批次检测出毛两面针素,存在用两面针混伪品投料生产的情况。结论:本方法简便、快速、准确。建立的检测方法可快速进行金鸡片中毛两面针素的定性检测。

Objective： To identify toddalolactone and establish the analysis method for Jinji tablets. Methods： An Hypersil DBS C18 column（250 mm × 4.6 mm,5μm） was used. The mobile phase consisted of acetonitrile-0.1% phosphoric acid solution. The flow rate was 0.8 ml·min -1 and the detection wavelength was at 330 nm. Toddalolactone was identified by an LC-MS method and the result was compared with that of the reference regent. TLC and HPLC analytical methods were used for analysis of toddalolactone. Results： Totally 58 batches of Jinji tablets were tested, and the shspected samples were confirmed by HPLC-MS/MS. Toddalolactone was detected out from 20 batches of samples. Conclusion： The method is simple, rapid and accurate, which is able to detect toddalolactone quickly and effectively.