HPLC法同时测定元胡止痛滴丸中6种成分

Simultaneous determination of six ingredients in Yuanhu Zhitong Dripping Pills by HPLC

目的建立同时测定元胡止痛滴丸中6种成分的HPLC分析方法。方法色谱柱为Diamonsil C18柱（250 mm×4.6mm,5μm）;流动相为乙腈-0.04%乙酸铵溶液（冰醋酸调p H值至4.0）,梯度洗脱：0~10 min,20%乙腈;10~25 min,20%~25%乙腈;25~70 min,25%~75%乙腈;体积流量1 m L/min;柱温35℃;检测波长280 nm;进样量10μL,测定元胡止痛滴丸中延胡索乙素、黄藤素、去氢延胡索甲素、延胡索甲素、欧前胡素和异欧前胡素的量。结果延胡索乙素、黄藤素、去氢延胡索甲素、延胡索甲素、欧前胡素和异欧前胡素分离度良好,阴性无干扰,分别在14.94~149.40、1.97~19.72、15.94~159.36、9.72~97.20、2.82~28.17、0.61~6.06μg/m L线性关系良好,r均大于0.999 0,平均加样回收率为95%~105%（RSD1.82%~2.99%）。4批样品中延胡索乙素、黄藤素、去氢延胡索甲素、延胡索甲素、欧前胡素、异欧前胡素的量分别在0.368~0.483、0.058~0.082、0.532~0.766、0.315~0.459、0.145~0.212、0.030~0.053 mg/g。结论方法简便、准确,重复性好,适用于元胡止痛滴丸中6种成分的定量测定,可为元胡止痛滴丸的质量控制提供依据。

Objective To establish a method of HPLC for simultaneous determination of six ingredients in Yuanhu Zhitong Dripping Pills. Methods Separation was performed on a Diamonsil C18 column（250 mm × 4.6 mm, 5 μm）; Mobile phase was acetonitrile（A）-0.04% ammonium acetate（acetic acid tone p H 4.0）（B）, gradient elution： 0—10 min, 20% A, 10—25 min, 20%—25% A, 25—70 min, 25%—75% A; flow rate was 1 m L/min; column temperature was 35 ℃; detection wavelength was 280 nm; and injection volume was 10 μL. The contents of dl-tetrahydropalmatine, palmatine, dehydrocorydaline, d-corydaline, imperatorin, and isoimperation were determined. Results The linear ranges were 14.94 — 149.40 μ g/m L for dl-tetrahydropalmatine, 1.97 — 19.72 μ g/m L for palmatine, 15.94 — 159.36 μ g/m L for dehydrocorydaline, 9.72 — 97.20 μ g/m L for d-corydaline, 2.82 — 28.17 μ g/m L for imperatorin, and 0.61 — 6.06 μ g/m L for isoimperation,respectively, with the correlation r 〉 0.999 0. The extraction recoveries varied from 95% to 105%（RSD varied from 1.82% to 2.99%）.The contents of dl-tetrahydropalmatine, palmatine, dehydrocorydaline, d-corydaline, imperatorin, and isoimperation was 0.368 —0.483, 0.058—0.082, 0.532—0.766, 0.315—0.459, 0.145—0.212, and 0.030—0.053 mg/g, respectively. Conclusion The method is accurate and reliable, which can be used for the quality control of Yuanhu Zhitong Dripping Pills.