华蟾素肠溶胶囊中5-羟色胺溶出度测定方法考察

Study on dissolution determination method of 5-hydroxytryptamine in cinobufotalin enteric capsule

目的建立华蟾素肠溶胶囊中5-羟色胺的体外溶出度测定方法。方法将4粒华蟾素胶囊样品加入到100 mL溶出杯中,溶出介质分别为0.1 mol·L^(-1)盐酸溶液(模拟胃液)和酸碱度(pH)6.8磷酸盐缓冲液(模拟肠液),溶出介质体积100 mL,将溶出杯置于全自动溶出试验仪,溶出温度(37.0±0.5)℃,仪器转速100 r·min^(-1),样品于0.1 mol·L^(-1)盐酸溶液和pH 6.8磷酸盐缓冲液中的取样时间分别为2 h和30 min。采用紫外-可见分光光度法检测华蟾素肠溶胶囊中5-羟色胺在0.1 mol·L^(-1)盐酸溶液和pH 6.8磷酸盐缓冲液中的溶出度。对本研究所建立的华蟾素肠溶胶囊中5-羟色胺的体外溶出度测定方法进行精密度、重复性及回收率考察。结果5-羟色胺对照品浓度在4.802~21.008 mg·L^(-1)范围内与吸光度值呈良好的线性关系。华蟾素肠溶胶囊中5-羟色胺在0.1 mol·L^(-1)的盐酸溶液中的溶出度为(0.04±0.03)%,在磷酸盐缓冲液(pH 6.8)中的溶出度为(84.6±1.9)%。本研究所建立的华蟾素肠溶胶囊中5-羟色胺的体外溶出度测定方法,精密度试验相对标准偏差(RSD)为0.76%。华蟾素肠溶胶囊在0.1 mol·L^(-1)的盐酸溶液中5-羟色胺溶出度重复性测定的RSD为0.04%,在pH 6.8磷酸盐缓冲液中重复性测定的RSD为2.9%,重复性良好。华蟾素肠溶胶囊在pH 6.8磷酸盐缓冲液中5-羟色胺的回收率为97.47%,RSD为1.6%。结论本研究所建立的华蟾素肠溶胶囊中5-羟色胺的体外溶出度测定方法使华蟾素肠溶胶囊中5-羟色胺在模拟胃液中的溶出度不超过10%,在模拟肠液中的溶出度不低于70%,精密度、重复性良好,回收率高,可为华蟾素胶囊的质量控制提供参考。

Objective To establish a dissolution rate determination method of 5-hydroxytryptamine in cinobufotalin enteric capsule in vitro.Methods Four cinobufacini enteric capsule samples were added to a 100 mL dissolution vessel,and the dissolution medium was 0.1 mol·L^(-1) hydrochloric acid solution(simulated gastric juice)and hydrogen ion concentration(pH)6.8 phosphate buffer(simulated intestinal juice),and the volume of the dissolution medium was 100 mL,and the dissolution vessel was placed in an automatic dissolution tester.The dissolution temperature was(37.0±0.5)℃,and the instrument speed was 100 r·min^(-1).The time of the sample taken out in 0.1 mol·L^(-1) hydrochloric acid solution and pH 6.8 phosphate buffer is 2 h and 30 min,respectively.The dissolution rate of 5-hydroxytryptamine in cinobufotalin enteric capsule in 0.1 mol·L^(-1) hydrochloric acid solution and pH 6.8 phosphate buffer was detected by ultraviolet-visible spectrophotometry.The precision,repeatability and recovery rate of the dissolution rate determination method of 5-hydroxytryptamine in cinobufotalin enteric capsule in vitro established in this study were investigated.Results The concentration of 5-hydroxytryptamine reference substance in the range of 4.802-21.008 mg·L^(-1) showed a good linear relationship with the absorbance value.The dissolution rate of 5-hydroxytryptamine in cinobufotalin enteric capsule in 0.1 mol·L^(-1) hydrochloric acid solution was(0.04±0.03)%,and the dissolution rate in pH 6.8 phosphate buffer was(84.6±1.9)%.The relative standard deviation(RSD)of the precision test was 0.76%for the in vitro dissolution determination method of 5-hydroxytryptamine in cinobufotalin enteric capsule established in this study.The RSD of the reproducible determination of 5-hydroxytryptamine dissolution rate in cinobufotalin enteric capsule in 0.1 mol·L^(-1) hydrochloric acid solution was 0.04%,and in pH 6.8 phosphate buffer was 2.9%,and the repeatability was good.The recovery rate of 5-hydroxytryptamine in cinobufotalin enteric capsule in pH 6.8 phosphate buffer was 97.47%,and the RSD was 1.6%.Conclusion The dissolution determination method of 5-hydroxytryptamine in cinobufotalin enteric capsule in vitro established in this study makes the dissolution rate of 5-hydroxytryptamine in cinobufotalin enteric capsule in simulated gastric juice not more than 10%,and the dissolution rate in simulated intestinal fluid is not lower than 70%.It has good properties and high recovery rate,which can provide reference for the quality control of cinobufotalin enteric capsule.