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Rg_1、人参皂苷Rb_1、三七皂苷R_1、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,5.0μm);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1.0mL/min;柱温35℃。结果尿囊素、人参皂苷Rg_1、人参皂苷Rb_1、三七皂苷R_1、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)、1.2～120.0μg/mL(r=0.999 6)、1.2～120.0μg/mL(r=0.999 6)、0.4～40.0μg/mL(r=0.999 2)、4.0～400.0μg/mL(r=0.999 8)、0.4～40.0μg/mL(r=0.999 1)、0.16～16.0μg/mL(r=0.999 1)、0.08～8.00μg/mL(r=0.999 0)、0.2～20.0μg/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Rg_1、人参皂苷Rb_1、三七皂苷R_1、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。
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,5.0μm)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—160.0μg/mL(r=0.999 7),1.2—120.0μg/mL(r=0.999 6),1.2—120.0μg/mL(r=0.999 6),0.4—40.0μg/mL(r=0.999 2),4.0—400.0μg/mL(r=0.999 8),0.4—40.0μg/mL(r=0.999 1),0.16—16.0μg/mL(r=0.999 1),0.08—8.00μg/mL(r=0.999 0),and 0.2—20.0μg/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.
作者
杨帆
傅琳
YANG Fan;FU Lin(The Second Hospital of Tianjin Medical University,Tianjin 300210,China;Tianjin Institute of Pharmaceutical Research,Tianjin 300193,China)
出处
《中草药》
CAS
CSCD
北大核心
2019年第5期1117-1121,共5页
Chinese Traditional and Herbal Drugs
