HPLC法测定复方愈创木酚磺酸钾口服溶液中愈创木酚磺酸钾和盐酸异丙嗪的含量

Determination of potassium guaiacolsulfonate and promethazine hydrochloride in compound guaiacol potassium sulfonate oral solution by HPLC

目的:建立HPLC法同时测定复方愈创木酚磺酸钾口服溶液中愈创木酚磺酸钾和盐酸异丙嗪的含量。方法:色谱柱为Waters Sunfire C 18(4.6 mm×150 mm,5μm);以0.02 mol·L^-1磷酸二氢钾缓冲液(取磷酸二氢钾2.72 g、四丁基硫酸氢铵3.4 g,加水800 mL使溶解,用1 mol·L^-1磷酸氢二钾溶液调节pH值至3.5)-乙腈(75∶25)为流动相;流速:1 mL·min^-1,检测波长为280 nm(愈创木酚磺酸钾)、250 nm(盐酸异丙嗪),柱温为30℃,进样量为10μL。结果:愈创木酚磺酸钾在0.15~1.8 mg·mL^-1、盐酸异丙嗪在2.5~125μg·mL^-1范围内与峰面积均呈良好线性关系,分别为r=0.9999(n=5)、r=1.0000(n=5),愈创木酚磺酸钾平均回收率为101.8%,RSD%为1.56%(n=9),盐酸异丙嗪平均回收率为101.1%,RSD%为1.48%(n=9)。收集的13家生产企业25批样品,测得愈创木酚磺酸钾标示含量88.3%~100.8%,盐酸异丙嗪标示含量48.9%~96.1%。结论:本法能同时测定复方愈创木酚磺酸钾口服溶液中愈创木酚磺酸钾和盐酸异丙嗪的含量,专属准确,操作简便快捷,可用于复方愈创木酚磺酸钾口服溶液的质量控制。

Objective:To establish a HPLC method for determination of potassium guaiacolsulfonate and promethazine hydrochloride in compound Guaiacol Potassium Sulfonate Oral Solution.Methods:The analysis was achieved by using Waters Sunfire C 18 column with 0.02 mL·L^-1 potassium dihydrogen phosphate buffer solution(potassium dihydrogen phosphate 2.72 g and tetrabutylammonium hydrogen sulfate 3.4 g,add 800 mL of water to dissolve,the pH value adjusted by 1mol·L^-1 dipotassium hydrogen phosphate solution to pH 3.5)-acetonitrile(75∶25)as mobile phase.The flow rate was 1mL·min^-1.The UV-detector at wavelength 280 nm(potassium guaiacolsulfonate)and 250 nm(promethazine hydrochloride).The column temperature is 30℃and the injection volume is 10μL.Results:The linear response ranges were:0.15-1.8 mg·mL^-1 for potassium guaiacolsulfonate(r=0.9999,n=5),2.5-125μg·mL^-1 for promethazine hydrochloride(r=1.0000,n=5)respectively.The mean recoveries of potassium guaiacolsulfonate and promethazine hydrochloride were 101.8%(RSD%=1.56%,n=9),101.1%(RSD%=1.48%,n=9)respectively.The labeled content of potassium guaiacolsulfonate were 88.3%to 100.8%,and the labeled content of promethazine hydrochloride were 48.9%to 96.1%of collected 25 batches of samples from 13 manufacturing companies.Conclusion:This method is simple,quick and the result of determination is precise of accurate.This method is suitable for determination of potassium guaiacolsulfonate and promethazine hydrochloride in compound preparation.