[关键词]
[摘要]
目的 建立HPLC法同时测定消风止痒颗粒中毛蕊花糖苷、焦地黄苯乙醇苷B1、升麻素苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、苍术素醇、白术内酯Ⅱ和苍术素,并采用化学计量学方法对检测结果进行综合评价。方法 采用Agilent Zorbax SB-C18色谱柱(250 mm×4.6 mm,5μm);以乙腈-0.2%磷酸溶液为流动相,梯度洗脱;检测波长:330 nm(0~14 min检测毛蕊花糖苷和焦地黄苯乙醇苷B1)、254 nm(14~31 min检测升麻素苷、升麻素、5-O-甲基维斯阿米醇苷和亥茅酚苷)、270 nm(31~55 min检测苍术素醇、白术内酯Ⅱ和苍术素);体积流量0.9 mL/min;柱温25℃;进样量10 μL。采用SPSS 26.0统计软件对消风止痒颗粒中9种成分进行聚类分析和主成分分析。结果 毛蕊花糖苷、焦地黄苯乙醇苷B1、升麻素苷、升麻素、5-O-甲基维斯阿米醇苷、亥茅酚苷、苍术素醇、白术内酯Ⅱ和苍术素分别在2.53~63.25、1.09~27.25、8.17~204.25、2.38~59.50、4.07~101.75、1.74~43.50、0.66~16.50、1.47~36.75、2.86~71.50μg/mL线性关系良好;平均回收率分别为99.01%、98.17%、100.13%、97.63%、98.72%、97.22%、96.93%、99.24%、100.01%,RSD值分别为1.42%、1.26%、0.72%、1.55%、0.84%、1.06%、1.18%、0.67%、0.95%;11批样品聚类分析为3类,主成分1~3是影响消风止痒颗粒质量评价的主要因子。结论 该方法操作简便、重复性好,可作为消风止痒颗粒中多指标成分质量评价模式。
[Key word]
[Abstract]
Objective To establish an HPLC method for determination of verbascoside, jionoside B1, prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside, sec-O-glucosylhamaudol, atractylodinol, atracylenolide II, and atractylodin in Xiaofeng Zhiyang Granules, and combine chemometrics analysis to comprehensive evaluation of Xiaofeng Zhiyang Granules. Methods The Agilent Zorbax SB-C18 column (250 mm×4.6 mm, 5 μm) was used with acetonitrile-0.2% phosphoric acid solution as the mobile phase with gradient elution. The detection wavelength were set at 330 nm for verbascoside and jionoside B1, 254 nm for prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside, and sec-O-glucosylhamaudol, and 270 nm for atractylodinol, atracylenolide II, and atractylodin. The flow rate was set at 0.9 mL/min, column temperature was set at 25℃, and the injection volume was 10 μL. The cluster analysis and principal component analysis were conducted for the content results of nine constituents in Xiaofeng Zhiyang Granule by SPSS 26.0 statistical software. Results Verbascoside, jionoside B1, prim-O-glucosylcimifugin, cimifugin, 5-O-methylvisammioside, sec-O-glucosylhamaudol, atractylodinol, atracylenolide II, and atractylodin showed good linear relationships within the ranges of 2.53-63.25, 1.09-27.25, 8.17-204.25, 2.38-59.50, 4.07-101.75, 1.74-43.50, 0.66-16.50, 1.47-36.75, and 2.86-71.50 μg/mL, whose average recoveries were 99.01%, 98.17%, 100.13%, 97.63%, 98.72%, 97.22%, 96.93%, 99.24%, and 100.01% with the RSD values of 1.42%, 1.26%, 0.72%, 1.55%, 0.84%,1.06%, 1.18%, 0.67%, and 0.95%, respectively. The samples of 11 batches of Xiaofeng Zhiyang Granules were divided in to 3 categories. The principal component 1-3 was the main factor affecting the quality evaluation of Xiaofeng Zhiyang Granules. Conclusion The method is simple and repeatable, and can be used as an multi-index quality evaluation model for Xiaofeng Zhiyang Granules.
[中图分类号]
R286.02
[基金项目]
河南省重大科技专项(创新示范专项)项目(191110311100)