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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 HPLC method for the simultaneous determination of six components in Yuanhu Zhitong dropping pills. Methods The column was Diamonsil C18 (250 mm × 4.6 mm, 5 μm). The mobile phase consisted of acetonitrile-0.04% ammonium acetate solution (pH 4.0 with glacial acetic acid). The gradient elution was 0-10 min with 20% acetonitrile ; 10-25 min, 20-25% acetonitrile; 25-70%, 25-75% acetonitrile; volume flow rate 1 m L / min; column temperature 35 ° C .; detection wavelength 280 nm; injection volume 10 μL; Hu Zhitong pills in the tetrahydropalmatine, feline hormone, hydrogen hydrogen aesoline, faucet prime, imperatorin and isoimperatorin amount. Results The separation of tetrahydropalmatine, palmatine, tetrahydropalmatine, prometryne, imperatorin and isoimperatorin was good and negative without interference, respectively, at 14.94-149.40, 1.97-19.72 and 15.94-159.36 , 9.72 ~ 97.20,2.82 ~ 28.17 and 0.61 ~ 6.06μg / m L, respectively. The average r was more than 0.999 0 and the average recoveries ranged from 95% to 105% (RSD 1.82% -2.99%). The contents of tetrahydropalmatine, palmatine, dehydrotalcobal, prometryne, imperatorin and isoimperatorin in four batches of samples were respectively 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. Conclusion The method is simple, accurate and reproducible. It is suitable for the quantitative determination of 6 components in Yuanhu Zhitong dropping pills, which can provide the basis for the quality control of Yuanhu Zhitong dropping pills.