[关键词]
[摘要]
目的 建立止动颗粒UPLC指纹图谱,并测定其中3种成分的含量。方法 以黄芩苷为参照峰,建立11批样品的UPLC指纹图谱,采用Acquity HSS T3色谱柱(150 mm×2.1 mm,1.8 μm),流动相为0.1%甲酸水溶液-乙腈,梯度洗脱,体积流量0.3 mL/min,柱温40℃,检测波长254 nm,测定黄芩苷、栀子苷和芍药苷的含量。结果 建立了UPLC指纹图谱,鉴定了没食子酸、车叶草苷、去乙酰车叶草苷酸甲酯、绿原酸、京尼平1-β-D-龙胆双糖苷、栀子苷、芍药苷、白杨素-6-C-β-D-葡萄糖-8-C-α-L-阿拉伯糖苷、白杨素-6-C-α-L-阿拉伯吡喃糖-8-C-β-D-葡萄糖苷、白杨素-6-C-α-L-阿拉伯吡喃糖-8-C-β-D-葡萄糖苷异构体、黄芩苷、黄芩苷异构体、千层纸素A-7-O-葡萄糖醛酸苷、汉黄芩苷、汉黄芩素、五味子醇甲16个成分,11批制剂相似度达到0.98以上。黄芩苷、栀子苷、芍药苷分别在12.15~388.80 μg/mL、6.52~209.00 μg/mL、8.38~268.00 μg/mL线性关系良好,平均加样回收率(RSD)分别为100.98%(3.04%)、100.49%(0.60%)、100.55%(2.73%)。11批制剂中黄芩苷为7.46~12.40 mg/g,栀子苷为7.01~13.27 mg/g,芍药苷为7.68~12.76 mg/g。结论 该方法准确简单,稳定可靠,可用于止动颗粒质量控制。
[Key word]
[Abstract]
Objective To establish the UPLC fingerprints of Zhidong Granules (ZG) and determine the content of three constituents. Methods With baicalin as a reference peak, the UPLC fingerprints of 11 batches of samples were established. The analysis of ZG was performed on a 40℃ thermostatic Acquity HSS T3 column (150 mm×2.1 mm, 1.8 μm), with the mobile phase comprising of acetonitrile-0.1% formic acid flowing at 0.3 mL/min in a gradient elution manner, and the detection wavelength was set at 254 nm. Results The UPLC fingerprint was established and 16 components were identified (gallic acid, asperuloside, methyl deacetylcyrrhizin, chlorogenic acid, genipin 1-gentiobioside, geniposide, paeoniflorin, chrysin-6-C-β-D-glucopyranosyl-8-C-α-L-arabinopyranoside, chrysin-6-C-α-L-arabopylanose-8-C-β-D-glucoside or isomer, baicalin, baicalin isomer, oroxylin A-7-O-glucuronide, wogonoside, wogonin, and schizandrin). The similarity of 11 batches of preparations were at least 0.98. Baicalin, paeoniflorin, and geniposide showed good linear relationships within the ranges of 12.15-388.80 μg/mL, 6.52-209.00 μg/mL, and 8.38-268.00 μg/mL, whose average recoveries (RSD) were 100.98% (3.04%), 100.49% (0.60%), and 100.55% (2.73%), respectively. The content of baicalin in the 11 batches of preparations was between 7.46 and 12.40 mg/g, the content of geniposide was between 7.01 and 13.27 mg/g, and the content of paeoniflorin was between 7.68 and 12.76 mg/g. Conclusion The method is accurate, simple, stable, and reliable, and can be used for quality control of ZG.
[中图分类号]
[基金项目]
国家科技重大专项重大新药创制项目“面向国际的创新中药大平台建设”(2013ZX09402202)