HPLC法测定平肺口服液中5个成分的含量  

Determination of five components in Pingfei oral liquid by HPLC

作　　者：肖宏华 马长华[2] 赫军[3] 马秉智[3] 刘开玉 XIAO Hong-hua;MA Chang-hua;HE Jun;MA Bing-zhi;LIU Kai-yu(Beijing Chaoyang District Food and Drug Safety Monitoring Center,Beijing 100023,China;Beijing University of ChineseMedicine,Beijing 102488,China;China-Japan Friendship Hospital,Beijing 100029,China)

机构地区：[1]北京市朝阳区食品药品安全监控中心,北京100023 [2]北京中医药大学,北京102488 [3]中日友好医院,北京100029

出　　处：《药物分析杂志》2019年第3期531-538,共8页Chinese Journal of Pharmaceutical Analysis

摘　　要：目的:建立HPLC法测定平肺口服液中芥子碱、绿原酸、五味子醇甲、贝母素甲、贝母素乙的含量。方法:采用HPLC-DAD法,以乙腈(A)-0.1%磷酸溶液(B)为流动相进行梯度洗脱,流速1.0 mL·min^(-1),检测波长327 nm(0～40 min)、216 nm(40～80 min),测定芥子碱、绿原酸、五味子醇甲的含量;采用HPLC-ELSD法,以乙腈-0.1%二乙胺溶液(60∶40)为流动相,流速1.0 mL·min^(-1),ELSD漂移管温度85℃,载气体积流量2.0 L·min^(-1),利用MCX混合型阳离子交换小柱进行固相萃取,测定贝母素甲、贝母素乙的含量。结果:芥子碱、绿原酸、五味子醇甲、贝母素甲、贝母素乙进样量分别在0.027 92～0.335 0μg(r=0.999 9)、0.04044～0.4 853μg(r=0.999 9)、0.012 90～0.154 8μg(r=0.999 9)、0.3 081～3.081 0μg(r=0.999 9)、0.317 4～3.174 0μg(r=0.999 9)范围内线性关系良好,平均回收率分别为101.0%、103.1%、103.8%、93.8%、94.4%,RSD分别为1.2%、0.46%、0.83%、2.1%、1.8%(n=9)。结论:该方法简便、准确,专属性强,可用于该制剂的质量控制。Objective:To establish an HPLC method for determination of sinapine,chlorogenic acid,schisandrin,peimine and peiminine in Pingfei oral liquid. Methods:Sinapine,chlorogenic acid and schisandrin were determined by HPLC-DAD method. The mobile phase was acetonitrile(A)-0.1% phosphoric acid solution(B)with gradient elution,the flow-rate was 1.0 mL·min-1 and the detection wavelengths were 327 nm(0-40 min)and 216 nm(40-80 min). Peimine and peiminine were determined by HPLC-ELSD method. The mobile phase was acetonitrile-0.1%diethylamine solution(60∶40),the flow-rate was 1.0 mL·min-1,the temperature for the detector drift tube was85 ℃,and the gas flow-rate was 2.0 L·min-1. Mixed cation exchange(MCX)column was used for solid phase extraction(SPE). Results:The methods achieved good linearity in the ranges of 0.027 92-0.335 0 μg(r=0.999 9)for sinapine,0.0404 4-0.485 3 μg(r=0.999 9)for chlorogenic acid,0.012 90-0.154 8 μg(r=0.999 9)for schisandrin,0.3 081-3.081 0 μg(r=0.999 9)for peimine and 0.317 4-3.174 0 μg(r=0.999 9)for peiminine,respectively. The average recoveries(n=9)were 101.0%(RSD=1.2%),103.1%(RSD=0.46%),103.8%(RSD=0.83%),93.8%(RSD=2.1%)and 94.4%(RSD1.8%),respectively. Conclusion:The method is simple,accurate,specific and can be used for quality control of the preparation.

关 键 词：平肺口服液 芥子碱 绿原酸 五味子醇甲 贝母素甲 贝母素乙 MCX固相萃取 

分 类 号：R917[医药卫生—药物分析学]