高效液相色谱法同时测定龙胆泻肝胶囊中9个成分含量  

Simultaneous determination of nine components in Longdan Xiegan caplsules by HPLC

作　　者：陈海滨 CHEN Haibin(Fujian Institute for Food and Drug Quality Control,Fuzhou 350001,China)

机构地区：[1]福建省食品药品质量检验研究院,福州350001

出　　处：《中国药品标准》2022年第4期446-454,共9页Drug Standards of China

摘　　要：目的:建立同时测定龙胆泻肝胶囊中栀子苷、龙胆苦苷、甘草酸、柴胡皂苷B_(2)、柴胡皂苷B_(1)、甘草酸、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素含量的高效液相色谱方法。方法:采用Welch ultimate XB-C_(18)色谱柱(4.6 mm×250 mm,5μm),以乙腈-0.1%磷酸水溶液为流动相,梯度洗脱,流速为1.0 mL·min^(-1),检测波长为254 nm(栀子苷、龙胆苦苷、甘草酸、柴胡皂苷B_(2)、柴胡皂苷B_(1))、280 nm(黄芩苷、汉黄芩苷、黄芩素、汉黄芩素),柱温为30℃。结果:栀子苷、龙胆苦苷、甘草酸、柴胡皂苷B_(2)、柴胡皂苷B_(1)、黄芩苷、汉黄芩苷、黄芩素、汉黄芩素进样量分别在0.0239~1.1940(r=0.9999)、0.0164~0.8201(r=0.9999)、0.0035~0.1725(r=0.9999)、0.0014~0.0679(r=0.9998)、0.0008~0.0377(r=0.9998)、0.0196~0.9582(r=1.0000)、0.0066~0.3308(r=0.9999)、0.0036~0.1810(r=0.9999)、0.0020~0.0999μg(r=1.0000)与峰面积呈良好的线性关系;定量下限分别为1.2、0.4、1.7、1.4、0.8、0.1、0.5、0.8、0.4 ng,平均回收率(n=9)分别为97.4%、100.8%、100.9%、99.3%、98.3%、99.3%、98.9%、98.0%、98.4%,RSD均小于3.8%,重复性RSD(n=6)均小于2.3%。含量测定结果表明,两个生产企业之间各成分的含量、比值1(黄芩苷/黄芩素)以及比值2(汉黄芩苷/汉黄芩素)差异较大。结论:经方法学验证,本法适用于龙胆泻肝胶囊整体质量评价。Objective:To develop an HPLC method for simultaneous determination of geniposide,gentiopicroside,glycyrrhizic acid,saikosaponin B_(1),saikosaponin B_(2),baicalin,wogonoside,baicalein and wogoni in Longdan Xiegan caplsules.Methods:The Welch ultimate XB C_(18) column(4.6 mm×250 mm,5μm)was adopted.The mobile phase was acetonitrile(A)-0.1% phosphoric acid aqueous solution(B),with a gradient elution.The flow rate was 1.0 mL·min^(-1).The detection wavelength was set at 254 nm for geniposide,gentiopicroside,glycyrrhizic acid,saikosaponin B_(2),saikosaponin B_(1).280 nm for baicalin,wogonoside,baicalein and wogoni.The column temperature was maintained at 30℃.Results:The calibration curves were linear in the quality range of 0.0239-1.1940μg(r=0.9999)for geniposide,0.0164-0.8201(r=0.9999)for gentiopicroside,0.0035-0.1725(r=0.9999)for glycyrrhizic acid,0.0014-0.0679(r=0.9998)for saikosaponin B_(2),0.0008-0.0377(r=0.9998)for saikosaponin B_(1),0.0196-0.9582(r=1.0000)for baicalin,0.0066-0.3308(r=0.9999)for wogonoside,0.0036-0.1810(r=0.9999)for baicalein,0.0020-0.0999μg(r=1.0000)for wogoni,the limits of quantitation were 1.2,0.4,1.7,1.4,0.8,0.1,0.5,0.8,0.4 ng.The average recoveries(n=9)were 97.4%,100.8%,100.9%,99.3%,98.3%,99.3%,98.9%,98.0% and 98.4% respectively.RSDs were less than 3.8% for the nine components.The RSDs of reproducibility(n=6)were less than 2.3%.The results of determination,the ratio 1(baicalin to baicalein)and the ratio 2(wogonoside to wogoni)showed that the content of each component varies between the two production enterprises.Conclusion:This method is proved by methodology validation that it can be used for overall quality evaluation of Longdan Xiegan caplsules.

关 键 词：龙胆泻肝胶囊 双波长 梯度洗脱 多成分测定 HPLC 

分 类 号：R921.2[医药卫生—药学]