摘要
目的 建立HPLC同时测定清肺抑火片中栀子苷、芒果苷、黄芩苷、盐酸小檗碱、汉黄芩苷、黄芩素、芦荟大黄素、大黄酸、汉黄芩素、大黄素、白花前胡甲素、大黄酚、大黄素甲醚、白花前胡乙素14种成分含量的方法.方法 采用Titank C18(250 mm×4.6 mm,5 μm)色谱柱;以0.1％磷酸溶液(A)-乙腈(B)为流动相,梯度洗脱;检测波长:栀子苷为238 nm,芦荟大黄素、大黄酸、大黄素、大黄酚、大黄素甲醚、芒果苷为254nm,盐酸小檗碱为265 nm,黄芩苷、汉黄芩苷、黄芩素、汉黄芩素为280 nm,白花前胡甲素、白花前胡乙素为321 nm;流速为1.0 mL·min-1;柱温为35 ℃;进样量为10μL.结果 栀子苷、芒果苷、黄芩苷、盐酸小檗碱、汉黄芩苷、黄芩素、芦荟大黄素、大黄酸、汉黄芩素、大黄素、白花前胡甲素、大黄酚、大黄素甲醚、白花前胡乙素的线性范围分别为4.96～223.17,0.84～42.22,18.76～938.16,4.46～223.17,4.86～243.10,1.59～79.32,0.76～38.17,1.03～51.49,1.59～79.40,1.21～60.72,1.80～90.06,0.91～45.48,1.04～51.83,0.86～43.23 μg·mL-1,r均≥0.999 9.仪器精密度、稳定性、重复性试验的RSD均＜2％,平均加样回收率(n=6)均＞90％,RSD＜3％.结论 该方法操作简单,重复性好,可为完善清肺抑火片的质量标准提供科学依据.
Abstract
OBJECTIVE To establish a high-performance liquid chromatography method for the simultaneous determination of 14 components including geniposide,mangiferin,baicalin,berberine hydrochloride,wogonoside,baicalein,aloe-emodin,rhein,wogonin,emodin,praeruptorin A,chrysophanol,physcion and praeruptorin B in Qingfei Yihuo tablets.METHODS Titank C18(250 mm×4.6 mm,5 μm)column was used;0.1％phosphoric acid solution(A)-acetonitrile(B)was used as the mobile phase with gradient elution;detection wavelengths:geniposide at 238 nm,aloe-emodin,rhein,emodin,chrysophanol,physcion and mangiferin at 254 nm,berberine hydrochloride at 265 nm,baicalin,wogonoside,baicalein,and wogonin at 280 nm,praeruptorin A and praeruptorin B at 321 nm.The flow rate was 1.0 mL·min-1 and the column temperature was 35 ℃;the injection volume was 10 μL.RESULTS The linear ranges of geniposide,mangiferin,baicalin,berberine hydrochloride,wogonoside,baicalein,aloe-emodin,rhein,wogonin,emodin,praeruptorin A,chrysophanol,physcion and,praeruptorin B were 4.96-223.17,0.84-42.22,18.76-938.16,4.46-223.17,4.86-243.10,1.59-79.32,0.76-38.17,1.03-51.49,1.59-79.40,1.21-60.72,1.80-90.06,0.91-45.48,1.04-51.83 and 0.86-43.23 μg·mL-1,with r all≥0.999 9.The RSDs of instrument precision,stability and reproducibility tests were＜3％,and the average recoveries in sample(n=6)were＞90％,with the RSDs＜3％.CONCLUSION The method is simple and reproducible and can provide a scientific basis for improving the quality standard of Qingfei Yihuo tablets.
基金项目
云南省药品监督管理局评价抽检计划(云药监办20227号)
维普
万方数据