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机构地区:[1]北京市海淀区药品检验所,北京100083 [2]北京中医药大学第三附属医院,北京100029
出 处:《中成药》2011年第7期1186-1189,共4页Chinese Traditional Patent Medicine
摘 要:目的用高效液相色谱梯度洗脱法同时测定活血止痛胶囊(当归、三七、乳香、土鳖虫、冰片、自然铜)三七中三七皂苷R1、人参皂苷Rg1和人参皂苷Rb13种皂苷;用高效液相色谱法测定当归中阿魏酸,为制定该制剂质量标准中定量测定方法及限度提供依据。方法三七皂苷R1、人参皂苷Rg1和人参皂苷Rb13种皂苷色谱柱为kromasil TMC18分析柱;以乙腈-水梯度洗脱(0~12 min乙腈质量分数为19%;12~60 min乙腈质量分数由19%递升至36%);体积流量1 mL/min,检测波长203 nm,柱温25℃,进样量10μL;当归中阿魏酸色谱柱为kromasil TMC18分析柱;以乙腈-0.085%磷酸溶液(17∶83)为流动相,检测波长316 nm,柱温35℃,进样量10μL。结果三七皂苷R1、人参皂苷Rg1和人参皂苷Rb1的线性范围分别为0.922~5.534μg、1.337~8.021μg和1.032~6.182μg。平均加样回收率(n=6)分别为99.52%、99.66%和99.23%。阿魏酸线性范围分别为50.72~304.32μg。平均加样回收率(n=6)分别为99.32%。结论 HPLC梯度洗脱法能将多种皂苷很好地分离检测,提高了时效,减少了误差。结果表明,该方法简便可行、准确可靠,重现性好,结果稳定。可用于活血止痛胶囊中三七多种有效成分的测定。AIM To establish a method for determing notoginsenoside R1、ginsenoside Rg1、ginsenoside Rb1、 ferulic acid in Huoxue Zhitong Capsules(Angelicae sinensis Radix,Notoginseng Radix et Rhizoma,Olibarum,Eupolyphaga or steleophaga,Borneolum Syntheticm,Pyritum).METHODS The HPLC was carried out on kromasilTM C18 column with mobile phase of acetonitrile-water(0-12 min,19∶ 81;12-60 min,36∶ 64)for notoginsenoside R1,ginsenoside Rg1and ginsenoside Rb1.The flow rate was 1.0 mL/min at 25 ℃.The detection wavelength was set at 203 nm.The HPLC was carried out on kromasil TMC18 column with acetonitrile-0.085% phosphonic acid(17∶ 83)as mobile phase for ferulic acid,the detection wavelength was at 316 nm,the flow rate was 1.0 mL/min and the column temperature was maintained at 35 ℃.RESULTS The linearity of notoginsenoside R1、ginsenoside Rg1、and ginsenoside Rb1 was in the ranges of 0.922-5.534 μg,1.337-8.021 μg and 1.032-6.182 μg,respectively.Their average recoveries were 99.47%,99.02%and 99.12%,respectively.The linearity of ferulic acid was in the range of 50.72-304.32 μg.The average recovery was 99.32%.CONCLUSION The assay demonstrates that the method is simple,has adequate accuracy and selectivity to quantify the four active components in Huoxue Zhitong Capsules.
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