机构地区:[1]天津医科大学肿瘤医院药学部国家肿瘤临床医学研究中心天津市"肿瘤防治"重点实验室天津市恶性肿瘤临床医学研究中心,天津300060
出 处:《中草药》2016年第21期3824-3828,共5页Chinese Traditional and Herbal Drugs
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/LKH2P04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(,=0.9992)、10.09~151.31μg/mL(r=0.9992)、4.98-74.63μg/mL(r=0.9994)、2.05~30.74μg/mL(r=0.9996)、4.10~61.46μg/mL(r=0.9996)、2.93~43.98μg/mL(r=0.9993)、2.04~30.66μg/mL(r=0.9995)、12.54~181.55μg/mL(r=0.9997)、53.95-89.23μg/mL(r=0.9995)、12.05~180.68μg/mL(r=0.9995)、5.97~89.51μg/mL(r=0.9994)、7.99~119.82μg/mL(r=0.9996),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5-0-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、0Objective 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, 5μm) 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 2.08-31.22 μg/mL (r = 0.999 5), 4.01-60.15 μg/mL (r = 0.999 2), 10.09-151.31 μg/mL (r = 0.999 2), 4.98-74.63 μg/mL (r = 0.999 4), 2.05-30.74 μg/mL (r = 0.999 6), 4.10-61.46 μg/mL (r = 0.999 6), 2.93-43.98 μg/mL (r = 0.999 3), 2.04-30.66 μg/mL (r = 0.999 5), 12.54-181.55 μg/mL (r = 0.999 7), 53.95-89.23 μg/mL (r =0.999 5), 12.05-180.68 μg,/mL (r = 0.999 5), 5.97-89.51 μg/mL (r= 0.999 4), and 7.99-119.82 μg/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 0.229-0.259 mg/L, 1.231-1.260 mg/L, 0.849-0.877 mg/L, 0.357-0.371 mg/L, 0.149-0.169 mg/L, 0.941-0.967 mg/L, 0.529-0.547 mg/L, 0.2
关 键 词:九味羌活口服液 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 5-O-甲基维斯阿米醇苷 RP—HPLC
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