HPLC同时测定喘舒片中的9种成分

Simultaneous determination of nine constituents in Chuanshu tablets by HPLC

目的采用HPLC波长切换法同时测定喘舒片中盐酸克仑特罗、黄芩苷、黄芩素、汉黄芩素、芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚的含量。方法采用Agilent TC-C_(18)(2)色谱柱(250 mm×4.6 mm,5μm),流动相为甲醇-0.1%磷酸溶液,梯度洗脱,检测波长分别为245、278、254 nm,流速1.0 mL·min^(-1),柱温35℃。结果盐酸克仑特罗、黄芩苷、黄芩素、汉黄芩素、芦荟大黄素、大黄酸、大黄素、大黄酚和大黄素甲醚的线性范围分别为0.92~18.28(r=0.9989)、63.75~1275(r=0.9999)、11.07~221.4(r=0.9996)、6.07~121.40(r=0.9995)、1.20~24.10(r=0.9998)、1.20~24.08(r=0.9994)、2.08~24.16(r=0.9999)、2.89~57.88(r=0.9993)、1.79~35.80(r=0.9997)μg·mL^(-1);平均加样回收率分别为98.62%、100.02%、99.84%、97.35%、98.38%、98.92%、100.23%、99.84%、97.74%,RSD分别为1.28%、1.61%、0.78%、1.02%、2.57%、1.80%、1.53%、1.29%、2.42%;9种成份在样品中的含量分别为每片8.65×10^(-3)~0.01104、49.460~57.464、0.864~1.883、0.215~0.388、0.0371~0.0866、0.0399~0.131、0.0464~0.0916、0.143~0.327、0.154~0.267 mg。结论所用方法简便、准确、重复性好,灵敏度高,可用于喘舒片的质量控制。

OBJECTIVE To establish an HPLC wavelength switching method to determine the content of clenbuterol hydrochloride,baicalin,baicalein,wogonin,aloe-emodin,rhein,emodin,chrysophanol and physcion in Chuanshu tablets simultaneously.METHODS The analysis of methanol extract of this drug was performed on Agilent TC-C_(18)(2)(250 mm×4.6 mm,5μm)column.The mobile phase was methanol-0.1%H3PO4 solution with gradient elution.The detection wavelengths were 245,278 and 254 nm.The flow rate was 1.0 mL·min^(-1),and the temperature of column was 35℃.RESULTS Clenbuterol hydrochloride,baicalin,baicalein,wogonin,aloe-emodin,rhein,emodin,chrysophanol and physcion showed good linear relationships within the ranges of 0.92-18.28μg·mL^(-1)(r=0.9989),63.75-1275μg·mL^(-1)(r=0.9999),11.07-221.4μg·mL^(-1)(r=0.9996),6.07-121.40μg·mL^(-1)(r=0.9995),1.20-24.10μg·mL^(-1)(r=0.9998),1.20-24.08μg·mL^(-1)(r=0.9994)、2.08-24.16μg·mL^(-1)(r=0.9999),2.89-57.88μg·mL^(-1)(r=0.9993),and 1.79-35.80μg·mL^(-1)(r=0.9997).The average recoveries were 98.62%,100.02%,99.84%,97.35%,98.38%,98.92%,100.23%,99.84%and 97.74%,with the RSDs of 1.28%,1.61%,0.78%,1.02%,2.57%,1.80%,1.53%,1.29%and 2.42%,respectively.The contents of clenbuterol hydrochloride,baicalin,baicalein,wogonin,aloe-emodin,rhein,emodin,chrysophanol and physcion were 8.65×10^(-3)-0.01104,49.460-57.464,0.864-1.883,0.215-0.388,0.0371-0.0866,0.0399-0.131,0.0464-0.0916,0.143-0.327,and 0.154-0.267 mg in one tablet,respectively.CONCLUSION The established method is simple and accurate,with a good reproducibility and high sensitivity.It can be used for the quality control of Chuanshu tablets.