复方苦参注射液总糖纯化方法及含量测定研究

Research on Purification Method and Determination of Total Sugar in Compound Kushen Injection

目的:建立复方苦参注射液总糖纯化及含量测定方法。方法:以单因素考察对复方苦参注射液总糖纯化条件进行优选,以苯酚-硫酸法测定复方苦参注射液中总糖含量。结果:复方苦参注射液总糖纯化条件:复方苦参注射液1 mL,稀释5倍,在床容积(BV)为15 mL的AB-8大孔吸附树脂柱进行上样,用3BV水洗脱,洗脱流速为0.566 mL/cm^(2)·min,得滤出液;苯酚硫酸法测定复方苦参注射液总糖专属性良好,浓度在28.06~92.18μg/mL范围内线性关系良好,r=0.9997,样品精密度、重复性、稳定性、耐用性RSD分别为0.02%、1.51%、0.72%、0.31%,加样回收率为96.84%~104.46%。结论:采用大孔吸附树脂纯化复方苦参注射液中的总糖准确可靠,用苯酚-硫酸方法测定复方苦参注射液中的总糖快速准确,可作为复方苦参注射液总糖纯化、测定方法。

Objective This study was to optimize the purification method of total sugar and establish a method for determining the total sugar in Compound Kushen Injection.Methods The conditions for purification of total sugar in Compound Kushen Injection were optimized by single factor investigation.The total sugar content in Compound Kushen Injection was determined by phenol-sulfuric acid method.Results The purification conditions of total sugar in compound Kushen injection:1 mL of compound Kushen injectionwasdiluted 5 times and loaded on an AB-8 macroporous adsorption resin column with a bed volume(BV)of 15 mL,which was eluted with triple times BV of water.The elution flow rate is 0.566 mL/cm^(2)·min,and the filtrate was obtained.The phenol-sulfuric acid method has a good specificity for determining the total sugar content in the compound injection,and the linear relationship is good within the range of 28.06 to 92.18μg/mL.The RSD of precision,repeatability,stability,and durability was 0.02%,1.51%,0.72%,and 0.31%,respectively,and the sample recovery rate was 96.84%to 104.46%.Conclusion The methods of macroporous adsorption resin purification and phenol-sulfuric acid determination in this study were accurate,reliable and rapid,which can be applied in the purification and determination of total sugar in compound Kushen injection.