黄芪赤风汤指纹图谱建立及主要成分含量测定

Establishment of Fingerprint and Determination of Main Components of Huangqi Chifeng Decoction(黄芪赤风汤)

目的 建立10批黄芪赤风汤供试品溶液的指纹图谱,以及对方中芍药内酯苷、芍药苷、毛蕊异黄酮葡萄糖苷、芒柄花苷、毛蕊异黄酮、芒柄花素、黄芪甲苷7种主要成分进行测定。方法 采用Diamonsil C18(2)色谱柱(4.6 mm×250 mm,5μm);使用0.05%甲酸水(B)-5%四氢呋喃95%乙腈(D)为流动相进行梯度洗脱;流量:1 mL/min;柱温:23℃,进样量:10μL。基于HPLC-ELSD法,漂移管温度:60℃,柱温:30℃,进样量:20μL。结果 10批黄芪赤风汤供试品共标出16个共有峰,其相似度均在0.9以上,并对毛蕊异黄酮葡萄糖苷、芒柄花素、芍药苷、升麻素、5-O-甲基维斯阿米醇苷、毛蕊异黄酮、芍药内酯苷分别进行指认;基于HPLC-ELSD法:10批黄芪赤风汤其相似度均在0.903以上。且7种主要成分在各自的加样范围中线性关系良好,各自加样回收率RSD≤3%,含量为:芍药内酯苷(9.58±1.70)mg/g、芍药苷(8.36±0.78)mg/g、毛蕊异黄酮葡萄糖苷(0.77±0.11)mg/g、芒柄花苷(0.16±0.06)mg/g、毛蕊异黄酮(0.50±0.06)mg/g、芒柄花素(0.25±0.05)mg/g、黄芪甲苷(0.30±0.10)mg/g。结论 本研究建立的黄芪赤风汤指纹图谱分析方法可信度高、稳定,可用于黄芪赤风汤的质量控制及含量测定。

Objective To establish the fingerprints of 10 batches of Huangqi Chifeng Decoction(黄芪赤风汤)test solution,as well as paeoniflorin,paeoniflorin,verbascoside,formononein,verbascoside,formononetin,and astragaloside IV in each other.7 main components were measured.Methods Use Diamonsil C18(2)column(4.6 mm×250 mm,5μm);use 0.05%formic acid water(B)-5%tetrahydrofuran 95%acetonitrile(D)as mobile phase for gradient elution;flow rate:1 mL/min;column temperature:23℃,injection volume:10μL.Based on HPLC-ELSD method,drift tube temperature:60℃,column temperature:30℃,injection volume:20μL.Results 10 batches of Huangqi Chifeng Decoction were marked with 16 common peaks,and their similarity was above 0.9.Methyl visamitol glycosides,isoflavones,and paeoniflorin were identified respectively;based on HPLC-ELSD method:the similarity of 10 batches of Huangqi Chifeng Decoction were all 0.878-1.000.And the 7 main components have a good linear relationship in their respective loading ranges,and the respective loading recoveries RSD≤3%.Flavonoid glycosides(0.77±0.11)mg/g,formononetin(0.16±0.06)mg/g,verbascoside(0.50±0.06)mg/g,formononetin(0.25±0.05)mg/g,astragaloside IV(0.30±0.10)mg/g.Conclusion The fingerprint analysis method of Huangqi Chifeng Decoction established in this study has high reliability and stability,and can be used for quality control and content determination of Huangqi Chifeng Decoction.