目的 建立HPLC法同時測定十味降糖顆粒中毛蕊異黃酮葡萄糖苷、芒柄花素、新芒果苷、芒果苷、異芒果苷、3'-羥基葛根素、葛根素、3'-甲氧基葛根素、東莨菪素和東莨菪苷的方法，采用化學(xué)計量學(xué)對其進行分析。方法 采用SepaxBio C₁₈色譜柱（250 mm×4.6 mm，5 μm）；流動相為乙腈–0.1%甲酸，梯度洗脫；檢測波長254 nm（0～45 min測定毛蕊異黃酮葡萄糖苷、芒柄花素、新芒果苷、芒果苷、異芒果苷、3'-羥基葛根素、葛根素、3'-甲氧基葛根素）、346 nm（45～75 min測定東莨菪素和東莨菪苷）；柱溫30 ℃；體積流量1.0 mL/min；進樣10 μL。采用聚類分析、主成分分析、偏最小二乘法–判別分析法對10種成分測定結(jié)果進行評價。結(jié)果 毛蕊異黃酮葡萄糖苷、芒柄花素、新芒果苷、芒果苷、異芒果苷、3'-羥基葛根素、葛根素、3'-甲氧基葛根素、東莨菪素和東莨菪苷分別在1.97～98.50、3.43～171.50、12.35～617.50、6.28～314.00、0.56～28.00、3.99～199.50、15.46～773.00、3.05～152.50、0.43～21.50、0.77～38.50 μg/mL有良好的線性關(guān)系。平均回收率分別為98.54%、99.63%、100.09%、98.94%、97.11%、99.72%、100.06%、98.71%、96.97%、97.84%，RSD值分別為1.02%、0.84%、0.70%、1.26%、1.36%、0.69%、0.88%、1.42%、1.58%、1.79%。偏最小二乘–判別分析的分類結(jié)果與聚類分析的結(jié)果基本一致；芒柄花素（VIP＝1.575）、東莨菪苷（VIP＝1.516）、毛蕊異黃酮葡萄糖苷（VIP＝1.223）和葛根素（VIP＝1.095）可能是影響十味降糖顆粒產(chǎn)品質(zhì)量的主要潛在標(biāo)志物。結(jié)論 建立的方法準(zhǔn)確易行，為十味降糖顆粒多指標(biāo)成分質(zhì)量控制方法的制訂提供參考。

Objective To establish an HPLC method for simultaneous determination of calycosin 7-O-β-D-glucopyranoside,formononetin,neomangiferin,mangiferin,isomangiferin,3'-hydroxy puerarin,puerarin,3'-methoxy puerarin,scopoletin,and scopolin in Shiwei Jiangtang Granules,and to analyze the data by chemometric methods.Methods The separation was carried out on SepaxBio C₁₈column (250 mm×4.6 mm,5 μm).The mobile phase consisted of acetonitrile-0.1% formic acid with gradient elution.The detection wavelengths were set at 254 nm (for calycosin 7-O-β-D-glucopyranoside,formononetin,neomangiferin,mangiferin,isomangiferin,3'-hydroxy puerarin,puerarin,3'-methoxy puerarin) and 346 nm (for scopoletin and scopolin).The column temperature was 30℃,the volume flow was 1.0 mL/min,and the injection volume was 10 μL.Cluster analysis,principal component analysis,partial least squares-discriminant analysis method were used to evaluate the results of ten components.Results Calycosin 7-O-β-D-glucopyranoside,formononetin,neomangiferin,mangiferin,isomangiferin,3'-hydroxy puerarin,puerarin,3'-methoxy puerarin,scopoletin,and scopolin had good linear relationships within the ranges of 1.97-98.50,3.43-171.50,12.35-617.50,6.28-314.00,0.56-28.00,3.99-199.50,15.46-773.00,3.05-152.50,0.43-21.50,and 0.77-38.50 μg/mL.The average recoveries were 98.54%,99.63%,100.09%,98.94%,97.11%,99.72%,100.06%,98.71%,96.97%,and 97.84% with RSD values of 1.02%,0.84%,0.70%,1.26%,1.36%,0.69%,0.88%,1.42%,1.58%,and 1.79%,respectively.The classification results of partial least squares-discriminant analysis were basically consistent with those of cluster analysis.Formononetin (VIP=1.575),scopolin (VIP=1.516),calycosin 7-O-β-D-glucopyranoside (VIP=1.223) and puerarin (VIP=1.095) may be the main potential marker affecting the quality of Shiwei Jiangtang Granules.Conclusion The established HPLC method is convenient and accurate,which can be used for multi-index quality control for Shiwei Jiangtang Granules.

R286.02

山東省中醫(yī)藥科技發(fā)展計劃項目(2019-0449)