一测多评法同时测定新敷愈散中6种成分含量

Simultaneous determination of 6 components in Xinfuyu powder by QAMS

目的建立一测多评法同时测定新敷愈散中大黄素、盐酸小檗碱、盐酸黄柏碱、苍术素、芦丁和绿原酸的含量。方法运用HPLC法,以Diamonsil C_(18)(250 mm×4.6 mm,5μm)为色谱柱,以乙腈-0.1%磷酸溶液为流动相进行梯度洗脱,柱温30℃,检测波长230 nm,流速1.0 mL·min^(-1),进样量10μL;以盐酸小檗碱为内标物,建立盐酸小檗碱与其他5种成分的相对校正因子,并计算各成分含量。结果大黄素、盐酸小檗碱、盐酸黄柏碱、苍术素、芦丁和绿原酸分别在6.72~33.60、10.80~54.00、4.97~24.87、8.76~43.80、4.40~22.00、10.49~52.48μg·mL^(-1)内与峰面积线性关系良好;平均加样回收率为98.00%~104.79%,RSD值均小于3.0%;大黄素、盐酸黄柏碱、苍术素、芦丁和绿原酸相对校正因子分别为1.158、6.172、1.633、3.746、3.134;一测多评法计算值与外标法实测值间差异无统计学意义(P>0.05)。结论建立的一测多评法科学合理、稳定可行,可用于测定新敷愈散中6种成分含量,也为深入开展该制剂质量标准研究提供科学依据。

Objective To simultaneously determine emodin,berberine hydrochloride,phellodendrine hydrochloride,atractylodin,rutin and chlorogenic acid in Xinfuyu powder.Methods HPLC method were used performed on Diamonsil C_(18)(250 mm×4.6 mm,5μm).The chromatographic column is gradient elution acetonitrile-0.1%phosphoric acid solution was used as the mobile phase,and the column temperature was 30℃.The detection wavelength was 230 nm and the flow rate was 1 mL·min^(-1).While the injection volume was 10μL with berberine hydrochloride as the internal standard.The relative correction factors of the 6 components were established,and the content of each component was calculated.Results The linearity of emodin,berberine hydrochloride,phellodendrine hydrochloride,atractylodin,rutin and chlorogenic acid showed good linearity at 6.72~33.60,and 10.80~54.00,4.97~24.87,8.76~43.80,4.40~22.00,and 10.49~52.48μg·mL^(-1).The average sample recovery range was 98.00%~104.79%,with the RSD<3.0%.The relative correction factors of emodin,phellodendrine hydrochloride,atractylodin,rutin and chlorogenic acid were 1.158,6.172,1.633,3.746 and 3.134 respectively.There was no significant difference between the calculated values by QAMS method and the measured values by ESM(P>0.05).Conclusion The method is stable,reasonable,and feasible,which can be used to determine the content of 6 components in Xinfuyu powder and provide reference for further quality control.