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[摘要]
目的 建立HPLC-DAD法同时测定九味肝泰胶囊中尿囊素、人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1、黄芩苷、五味子醇甲、姜黄素、大黄素和大黄酚的方法。方法 采用HPLC法,色谱柱为Ultimate AQ-C18(150 mm×4.6 mm,5.0 μm);流动相为0.5%磷酸水溶液-(乙腈-甲醇20:80),梯度洗脱,体积流量1.0 mL/min;柱温35℃。结果 尿囊素、人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1、黄芩苷、五味子醇甲、姜黄素、大黄素和大黄酚9种成分能够达到良好分离;其线性范围分别为1.6~160.0μg/mL(r=0.999 7)、1.2~120.0 μg/mL(r=0.999 6)、1.2~120.0 μg/mL(r=0.999 6)、0.4~40.0 μg/mL(r=0.999 2)、4.0~400.0 μg/mL(r=0.999 8)、0.4~40.0 μg/mL(r=0.999 1)、0.16~16.0 μg/mL(r=0.999 1)、0.08~8.00 μg/mL(r=0.999 0)、0.2~20.0 μg/mL(r=0.999 2),平均加样回收率分别为99.3%、100.2%、99.8%、98.3%、99.9%、97.8%、97.8%、102.2%、101.9%,RSD分别为0.6%、0.5%、0.7%、1.1%、0.3%、0.9%、1.4%、1.5%、1.2%。9批次样品中尿囊素、人参皂苷Rg1、人参皂苷Rb1、三七皂苷R1、黄芩苷、五味子醇甲、姜黄素、大黄素和大黄酚质量浓度分别为3.634~3.655、2.523~2.611、2.405~2.424、0.802~0.829、10.362~10.623、0.901~0.921、0.334~0.366、0.142~0.160、0.462~0.479 mg/g。结论 本方法操作简便,测定结果准确可靠,可用于九味肝泰胶囊的质量控制。
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[Abstract]
Objective To establish HPLC-DAD method for the simultaneous determination of allantoin, ginsenoside Rg1, ginsenoside Rb1, notoginsenoside R1, baicalin, schisandrin, curcumin, emodin and chrysophanol in Jiuwei Gantai Capsules (JGC). Methods The chromatographic separation was achieved on an Ultimate AQ-C18 column (150 mm×4.6 mm, 5.0 μm) with mobile phase consisted of (0.1% phosphate)-(acetonitrile-methanol 20:80) for gradient elution, at the flow rate of 1.0 mL/min; The column temperature was 35℃. Results The linear ranges of allantoin, ginsenoside Rg1, ginsenoside Rb1, notoginsenoside R1, baicalin, schisandrin, curcumin, emodin, and chrysophanol were 1.6-160.0 μg/mL (r=0.999 7), 1.2-120.0 μg/mL (r=0.999 6), 1.2-120.0 μg/mL (r=0.999 6), 0.4-40.0 μg/mL (r=0.999 2), 4.0-400.0 μg/mL (r=0.999 8), 0.4-40.0 μg/mL (r=0.999 1), 0.16-16.0 μg/mL (r=0.999 1), 0.08-8.00 μg/mL (r=0.999 0), and 0.2-20.0 μg/mL (r=0.999 2), respectively. The average recoveries (n=6) were 99.3% (RSD=0.6%), 100.2% (RSD=0.5%), 99.8% (RSD=0.7%), 98.3% (RSD=1.1%), 99.9% (RSD=0.3%), 97.8% (RSD=0.9%), 97.8% (RSD=1.4%), 102.2% (RSD=1.5%), and 101.9% (RSD=1.2%), respectively. The content of the allantoin, ginsenoside Rg1, ginsenoside Rb1, notoginsenoside R1, baicalin, schisandrin, curcumin, emodin, and chrysophanol in nine batches were 3.634-3.655, 2.523-2.611, 2.405-2.424, 0.802-0.829, 10.362-10.623, 0.901-0.921, 0.334-0.366, 0.142-0.160, and 0.462-0.479 mg/g, respectively. Conclusion The method is accurate, sensitive, credible, and repeatable, which can be applied to the quality control of JGC.
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