高效液相色谱法同时测定黄芪赤风胶囊中芍药苷、升麻素苷等9种成分的含量

RP-HPLC Analysis of Nine Components in Huangqichifeng Capsules

目的建立HPLC同时测定黄芪赤风胶囊中9种成分的含量。方法采用Waters Symmetry Shield RP18(4.6 mm×150mm,5μm)色谱柱;以甲醇(A)-水溶液(B)为流动相进行梯度洗脱(0～15 min,5%A→20%A;15～55 min,20%A→35%A;55～100 min,35%A→85%A),流速1.0 mL·min-1;检测波长:230 nm(0～25 min,芍药苷),254 nm(25～100 min,毛蕊异黄酮苷等);柱温35℃。结果芍药苷、升麻素苷、毛蕊异黄酮苷、升麻素、5-O-甲基维斯阿米醇苷、芒柄花苷、亥茅酚苷、毛蕊异黄酮、芒柄花素的线性范围分别为1.51～15.10,0.047～0.94,2.192～10.960,0.052 2～1.044,0.041 4～0.828,1.56～7.80,0.042 2～0.844,0.149～0.744和0.110～0.552μg(r≥0.999 0);平均回收率(n=6)分别为99.48%(RSD=2.59%),103.15%(RSD=1.69%),102.77%(RSD=1.56%),99.27%(RSD=2.72%),101.99%(RSD=2.36%),102.25%(RSD=2.10%),101.49%(RSD=3.00%),100.45%(RSD=1.76%)和97.49%(RSD=2.03%)。结论所建立的方法快速、准确、专属性强、精密度好,可用于黄芪赤风胶囊的质量控制。

OBJECTIVE To develop an HPLC method for determination of nine components in Huangqichifeng capsules. METHODS The analysis was carded out on a Waters Symmetry Shield RPls column （4. 6 mm ×150 mm, 5 μm）. The mobile phase was composed of methanol （A） and water （B） with gradient elution （0- 15 min, 5% A→20% A; 15-55 min, 20% A→35% A; 55 - 100 min, 35% A→85% A） and the flow rate was 1.0 mL ·min^-1. The detection wavelengths were set at 230 nm for paeoniflorin （0-25 rain） and 254 nm for other components （25 - 100 min）. The column temperature was 35 ℃. RESULTS The linear ranges of paeoniflorin, prin-O-glucosylcimifugin, calycosin-7-O-β-D-glucopyranoside, eimifugin, 4＇-O-β-D-glucopyranosyl-5-O-methylvisammi- nol, formononetin-7-O-β-D-glucopyranoside, sec-O-glucosylhamaudol, calycosin, formononetin were 1. 510 - 15.1, 0. 047 - 0.94, 2. 192 - 10. 96, 0.052 2 - 1. 044, 0. 041 4 -0. 828, 1.56 -7.80, 0. 042 2 -0. 844, 0. 149 -0. 744 and 0. 110 -0. 552 μg （r≥ 0. 999 0） respectively. The average recoveries were 99.48% , 103.15%, 102.77%, 99. 27%, 101.99%, 102. 2.5% , 101.49%, 100.45% and 97.49% （RSD 〈2. 5% , n =6） respectively. CONCLUSION The method is simple, accurate, repeatable, and can be used to control the quality of Huangqichifeng capsules.