HPLC梯度洗脱法同时测定复方荆芥熏洗剂中的升麻素苷、5-O-甲基维斯阿米醇苷、齐墩果酸和熊果酸含量

目的采用高效液相梯度洗脱法建立复方荆芥熏洗剂中升麻素苷、5-O-甲基维斯阿米醇苷、齐墩果酸和熊果酸含量测定方法。方法 Hypersil C18色谱柱(4.6 mm×250 mm,5μm);流速:1.1 mL·min-1;流动相A为乙腈-甲醇(2:1),流动相B为1%冰醋酸溶液,梯度洗脱;检测波长分别为254 nm(升麻素苷和5-O-甲基维斯阿米醇苷)和205 nm(齐墩果酸和熊果酸)。结果升麻素苷、5-O-甲基维斯阿米醇苷、齐墩果酸和熊果酸分别在0.028 4⁰.568 0μg(r=0.999 7)、0.022 60.568 0μg(r=0.999 7)、0.022 6⁰.452 0μg(r=0.999 8)、0.010 80.452 0μg(r=0.999 8)、0.010 8⁰.216 0μg(r=0.999 3)、0.035 80.216 0μg(r=0.999 3)、0.035 8⁰.716 0μg(r=0.999 5)进样量与峰面积呈良好的线性关系,平均加样回收率分别为98.2%、98.0%、96.9%、97.7%,RSD(n=6)分别为0.85%、0.54%、0.93%、1.4%。结论方法简便、准确、灵敏、重复性好,可作为复方荆芥熏洗剂中升麻素苷、5-O-甲基维斯阿米醇苷、齐墩果酸和熊果酸的含量控制方法。

Determination of prim-O-glucosylcimifugin, 5-O-ethylvisammioside,oleanolic acid and ursolic acid in Fufang Jingjie lotion by HPLC

Objective To develop an HPLC method for the simultaneous determination of prim-O-glucosylcimifugin, 5-O-methylvisammioside, oleanolic acid and ursolic acid in Fufang Jingjie lotion. Methods The chromatograhic sepa- ration was performed on Hypersil C1＋ column, a linear elution of acetonitrile-methanol （2 ： 1） and 1% glacial acetic acid solution was adopted at the flow rate of 1.1 mL · min ^- 1. The UV detection wavelength were 254 nm for prim-O- glucosylcimifugin and 5-O-methylvisamrnioside, 205 mn for oleanolic acid and ursolic acid. Results Prim-O-glucosyl- cimifugin, 5-O-methylvisammioside, oleanolic acid and ursolic acid had good linearity at 0.028 4 - 0.568 0 μg （r = 0.999 7）, 0.022 6 - 0.452 0 μg （r = 0.999 8）, 0.010 8 - 0.216 0 μg （r = 0.999 3）, 0.035 8 - 0.716 0 μg （r = 0.999 5）, respectively. The average recoveries and RSD were 98.2% （0.85%）, 98.0% （0.54%）, 96.9% （0.93%） and 97.7% （1.4%）, respectively. Conclusion The method was convenient, accurate, sensitive, repetitive and may be used to determine the content of prim-O-glucosylcimifugin, 5-O-methylvisammioside, oleanolic acid and ursolic acid in Fufang Jingjie lotion.