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[摘要]
目的 建立RP-HPLC法同时测定九味羌活口服液(JQOL)中梓醇、甘草苷、甘草酸铵、细辛脂素、毛蕊花糖苷、苍术素、阿魏酸、欧前胡素、羌活醇、异欧前胡素、黄芩苷、升麻素苷和5-O-甲基维斯阿米醇苷的方法。方法 采用Zorbax Eclipse XDB-C18色谱柱(250mm×4.6mm,5μm);乙腈-5.0mmol/L KH2PO4溶液(稀磷酸调节pH值至3.0)(15∶85)为流动相,梯度洗脱,体积流量为1.0mL/min。结果 梓醇、甘草苷、甘草酸铵、细辛脂素、毛蕊花糖苷、苍术素、阿魏酸、欧前胡素、羌活醇、异欧前胡素、黄芩苷、升麻素苷和5-O-甲基维斯阿米醇苷13种成分能够达到很好分离;其线性范围分别为2.08~31.22μg/mL(r=0.9995)、4.01~60.15μg/mL(r=0.9992)、10.09~151.31μg/mL(r=0.999 2)、4.98~74.63μg/mL(r=0.999 4)、2.05~30.74μg/mL(r=0.999 6)、4.10~61.46μg/mL(r=0.999 6)、2.93~43.98μg/mL(r=0.999 3)、2.04~30.66μg/mL(r=0.999 5)、12.54~181.55μg/mL(r=0.999 7)、53.95~89.23μg/mL(r=0.999 5)、12.05~180.68μg/mL(r=0.999 5)、5.97~89.51μg/mL(r=0.999 4)、7.99~119.82μg/mL(r=0.999 6),平均加样回收率分别为98.8%、98.6%、101.2%、99.4%、100.1%、99.7%、98.9%、99.4%、100.5%、98.7%、101.2%、98.3%、99.1%,RSD分别为1.9%、1.8%、1.5%、0.8%、0.6%、0.9%、1.2%、2.0%、1.6%、0.8%、1.4%、1.5%、1.7%(n=6)。9批次JQOL供试品中梓醇、甘草苷、甘草酸铵、细辛脂素、毛蕊花糖苷、苍术素、阿魏酸、欧前胡素、羌活醇、异欧前胡素、黄芩苷、升麻素苷和5-O-甲基维斯阿米醇苷质量浓度分别为0.229~0.259mg/L、1.231~1.260mg/L、0.849~0.877mg/L、0.357~0.371mg/L、0.149~0.169mg/L、0.941~0.967mg/L、0.529~0.547mg/L、0.269~0.294mg/L、1.039~1.067mg/L、0.043~0.064mg/L、3.631~3.649mg/L、0.157~0.183mg/L、0.068~0.084mg/L。结论 该法分离度好,快速简便,重现性好,可用于JQOL的质量控制。
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[Abstract]
Objective To establish an HPLC method for the simultaneous determination of catalpol, liquiritin, ammonium glycyrrhizinate, asarinin, verbascoside, atractylodin, ferulic acid, imperatorin, notopterol, isoimperatorin, baicalin, prim- O-glucosylcimifugin, and 5- O-methylvisammioside in Jiuwei Qianghuo Oral Liquid (JQOL).Methods The analysis was performed on Zorbax Eclipse XDB- C18 column (250 mm × 4.6 mm, 5 μm) by gradient elution of acetonitrile-0.005 mol/L KH2PO4 (adjusting to pH 3.0 with phosphoric acid) (15:85). The flow rate was 1.0 mL/min.Results The linear ranges of catalpol, liquiritin, ammonium glycyrrhizinate, asarinin, verbascoside, atractylodin, ferulic acid, imperatorin, notopterol, isoimperatorin, baicalin, prim- O-glucosylcimifugin, and 5- O-methylvisammioside were 2.08—31.22μg/mL (r= 0.999 5), 4.01—60.15μg/mL (r= 0.999 2), 10.09—151.31μg/mL (r= 0.999 2), 4.98—74.63μg/mL (r= 0.999 4), 2.05—30.74μg/mL (r= 0.999 6), 4.10—61.46μg/mL (r= 0.999 6), 2.93—43.98μg/mL (r= 0.999 3), 2.04—30.66μg/mL (r= 0.999 5), 12.54—181.55μg/mL (r= 0.999 7), 53.95—89.23μg/mL (r= 0.999 5), 12.05—180.68μg/mL (r= 0.999 5), 5.97—89.51μg/mL (r= 0.999 4), and 7.99—119.82μg/mL (r= 0.999 6). The average recoveries (n= 6) were 98.8% (RSD= 1.9%), 98.6% (RSD= 1.8%), 101.2% (RSD= 1.5%), 99.4% (RSD= 0.8%), 100.1% (RSD= 0.6%), 99.7% (RSD= 0.9%), 98.9% (RSD= 1.2%), 99.4% (RSD= 2.0%), 100.5% (RSD= 1.6%), 98.7% (RSD= 0.8%), 101.2% (RSD= 1.4%), 98.3% (RSD= 1.5%), and 99.1% (RSD= 1.7%), respectively. The contents of nine batches of the catalpol, liquiritin, ammonium glycyrrhizinate, asarinin, verbascoside, atractylodin, ferulic acid, imperatorin, notopterol, isoimperatorin, baicalin, prim- O-glucosylcimifugin, and 5- O-methylvisammioside were 0.229—0.259mg/L, 1.231—1.260mg/L, 0.849—0.877mg/L, 0.357—0.371mg/L, 0.149—0.169mg/L, 0.941—0.967mg/L, 0.529—0.547mg/L, 0.269—0.294mg/L, 1.039—1.067mg/L, 0.043—0.064mg/L, 3.631—3.649mg/L, 0.157—0.183mg/L, and 0.068—0.084mg/L.Conclusion This method is simple and rapid, and can be used for the quality control of JQOL with satisfactory separation and repeatability.
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