摘要
目的建立HPLC-DAD法同时测定参芪十一味颗粒(SSG)中23-乙酰泽泻醇B、阿魏酸、毛蕊花糖苷、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、天麻素、大黄酚、橙黄决明素、毛蕊异黄酮葡萄糖苷和金丝桃苷的方法。方法采用RP-HPLC法,色谱柱为Waters XBridge-C18(250 mm×4.6 mm,5.0μm);流动相为甲醇-乙腈-水(15∶80∶5)和乙腈-0.1%磷酸水溶液(10∶90),梯度洗脱,体积流量1.0 m L/min;柱温35℃,进样量10μL。结果 23-乙酰泽泻醇B、阿魏酸、毛蕊花糖苷、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、天麻素、大黄酚、橙黄决明素、毛蕊异黄酮葡萄糖苷和金丝桃苷11种成分能够达到很好分离;其线性范围分别为0.4~8.0μg/m L(r=0.999 2)、0.2~4.0μg/m L(r=0.999 5)、0.2~4.0μg/m L(r=0.999 5)、0.1~2.0μg/m L(r=0.999 6)、0.1~2.0μg/m L(r=0.999 7)、0.1~2.0μg/m L(r=0.999 4)、0.5~10μg/m L(r=0.999 2)、0.6~12μg/m L(r=0.999 2)、0.4~8.0μg/m L(r=0.999 4)、1.0~20μg/m L(r=0.999 6)、0.8~16μg/m L(r=0.999 3),平均加样回收率分别为98.1%、98.1%、99.1%、98.3%、99.5%、99.9%、98.5%、100.4%、101.6%、99.7%、101.2%,RSD分别为0.9%、1.6%、1.6%、1.8%、1.5%、0.6%、0.7%、0.8%、0.4%、0.9%、1.1%(n=6)。9批次供试品中23-乙酰泽泻醇B、阿魏酸、毛蕊花糖苷、人参皂苷Rg1、人参皂苷Re、人参皂苷Rb1、天麻素、大黄酚、橙黄决明素、毛蕊异黄酮葡萄糖苷和金丝桃苷质量浓度分别为0.081~0.089、0.261~0.269、0.060~0.069、0.038~0.047、0.030~0.037、0.042~0.049、0.420~0.428、0.141~0.151、0.178~0.189、0.107~0.117、0.069~0.078 mg/g,结果表明本品各批次之间差异较小。结论本方法操作简便,测定结果准确可靠,可用于SSG的质量控制。
Objective To establish HPLC-DAD method for the simultaneous determination of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-Dglucopyranoside, and hyperoside in Shenqi Shiyiwei Granule(SSG). Methods The chromatographic separation was achieved on an Waters XBridge-C18(250 mm × 4.6 mm, 5.0 μm) column with methanol-acetonitrile-water(15∶80∶5) and methanol-0.1% phosphoric acid(10∶90) as mobile phases for gradient elution, at the flow rate of 1.0 m L/min; The column temperature was 35 ℃.Results The linear ranges of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside were 0.4—8.0 μg/m L(r = 0.999 2), 0.2—4.0 μg/m L(r = 0.999 5), 0.2—4.0 μg/m L(r = 0.999 5), 0.1—2.0 μg/m L(r = 0.999 6), 0.1—2.0 μg/m L(r = 0.999 7), 0.1—2.0 μg/m L(r = 0.999 4), 0.5—10 μg/m L(r = 0.999 2), 0.6—12 μg/m L(r = 0.999 2), 0.4—8.0 μg/m L(r = 0.999 4), 1.0—20 μg/m L(r = 0.999 6), and 0.8—16 μg/m L(r = 0.9993). The average recoveries(n = 6) were 98.1%(RSD = 0.9%), 98.1%(RSD = 1.6%), 99.1%(RSD = 1.6%), 98.3%(RSD = 1.8%), 99.5%(RSD = 1.5%), 99.9%(RSD = 0.6%), 98.5%(RSD = 0.7%), 100.4(RSD = 0.8%), 101.6%(RSD = 0.4%), 99.7%(RSD = 0.9%), and 101.2%(RSD = 1.1%), respectively. The contents of nine batches of 23-acetate alisol B, ferulic acid, verbascoside, ginsenoside Rg1, ginsenoside Re, ginsenoside Rb1, gastrodin, chrysophanol, aurantio-obtusin, calycosin 7-O-β-D-glucopyranoside, and hyperoside were 0.081—0.089, 0.261—0.269, 0.060—0.069, 0.038—0.047, 0.030—0.037, 0.042—0.049, 0.420—0.428, 0.141—0.151, 0.178—0.189, 0.107—0.117, and 0.069—0.078 mg/g. The results showed that there was little difference among the batches. Conclusion The method is accurate, sensitive, credible, and repeatable. It can be applied to the quality control of SSG.
出处
《中草药》
CAS
CSCD
北大核心
2017年第7期1344-1349,共6页
Chinese Traditional and Herbal Drugs