高效液相色谱-双波长紫外检测同时测定清肺抑火片中4种药效成分

Determination of four active components in Qingfei Yihuo Tablets by RP-HPLC

目的建立双波长RP-HPLC法同时测定清肺抑火片(黄芩、栀子、黄柏、大黄、苦参、天花粉等)中栀子苷、黄芩苷、盐酸小檗碱及大黄素4种药效成分。方法采用固定相为Eclipse XDB-C18柱(150 mm×4.6 mm,5μm);流动相为乙腈-0.2%磷酸水溶液进行梯度洗脱;体积流量1 mL/min;检测波长为240 nm(栀子苷),278 nm(黄芩苷、盐酸小檗碱、大黄素)。结果栀子苷、黄芩苷、盐酸小檗碱、大黄素进样量分别在0.036 8～0.331μg(r=0.999 8)、0.074 4～0.670μg(r=0.999 8)、0.038 7～0.348μg(r=0.999 9)、0.057 6～0.518μg(r=0.999 8)范围内与其峰面积积分值呈良好的线性关系,平均回收率依次为98.72%、98.69%、98.62%、98.56%,RSD(n=9)依次为1.17%、0.932%、1.16%、0.982%。结论本方法操作简便,准确度高,重现性和精密度均良好,可为清肺抑火片质量控制和评价提供一定的科学依据。

AIM To develop a reversed-phase HPLC method for determining four active components,including geniposide,baicalin,berberine hydrochloride and emodin in Qingfei Yihuo Tablets（Scutellariae Radix,Gardeniae Fructus,Phellodendri chinensis Cortex,Rhei Radix et Rhizoma,Sophorae flavescentis Radix,Trichosanthis Radix,etc.）.METHODS The determination was performed on a ZORBAX Eclipse XDB-C18 column（4.6 mm×150 mm,5 μm） with acetonitrile-0.2% phosphoric acid as the mobile phase in gradient elution mode at the flow rate of 1.0 mL/min.The detection wavelengths were set at 240 nm for geniposide and 278 nm for baicalin,berberine hydrochloride and emodin,respectively.The column temperature was maintained at 30 ℃.RESULTS Satisfactory linearities were obtained when the sample size of geniposide was between 0.036 8-0.331 μg（r=0.999 8,n=5）,of baicalin was between 0.074 4-0.670 μg（r=0.999 8,n=5）,of berberine hydrochloride was between 0.038 7-0.348 μg（r=0.999 9,n=5） and of emodin was between 0.057 6-0.518 μg（r=0.9998,n=5）,respectively.Their average recoveries were 98.72%,98.69%,98.62%,98.56%,respectively.CONCLUSION This proposed method is simple,accurate,reproducible and suitable for the determination of four components in Qingfei Yihuo Tablets,and can be also used for quality control and evaluation of the tablets.