[关键词]
[摘要]
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×4.6 mm,5 μm);流动相为乙腈-0.04%乙酸铵溶液(冰醋酸调pH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 mL/min;柱温35 ℃;检测波长280 nm;进样量10 μL,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、0.61~6.06 μg/mL线性关系良好,r均大于0.999 0,平均加样回收率为95%~105%(RSD 1.82%~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.
[Key word]
[Abstract]
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 pH 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 mL/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 μg/mL for dl-tetrahydropalmatine, 1.97-19.72 μg/mL for palmatine, 15.94-159.36 μg/mL for dehydrocorydaline, 9.72-97.20 μg/mL for d-corydaline, 2.82-28.17 μg/mL for imperatorin, and 0.61-6.06 μg/mL 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.
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[基金项目]
国家自然科学基金重点资助项目(81430096)