摘要
目的:建立高效液相色谱-蒸发光散射检测器(HPLC-ELSD)测定夜关门中D-松醇含量的方法。方法:样品用乙醇-水(70∶30)提取1.0 h后过滤,滤渣再用63%的乙醇-水提取1 h过滤,合并2次滤液并浓缩,定容;采用Cosmosil Sugar-D柱进行分离,乙腈-水(70∶30)为流动相,流速为1 mL·min-1,ELSD漂移管温度55℃,载气为氮气。结果:D-松醇在0.377~1.844μg呈现良好的线性关系(r=0.999 5),精密度为0.22%,加标回收率为96.78%。结论:该方法操作简单、准确度和灵敏度高、适合于D-松醇的检测和含量测定。
Objective:An analytical method was developed for determining D-pinitol in Lespedeza cuneata by HPLC-ELSD. Method : Sample was extracted by ethanol-water solution (70:30 by volume) for 1.0 h, then filtered and the residue was extracted by ethanol-water solution (63:37 by volume) for another hour, filtered again and combined the filtrate then concentrated it,and diluted it into 100 mL. The separation was performed on a Cosmosil-sugar D column with the mobile phase consisting of water and aeetonitrile (20:80 by volume). And the flow rate was 1 mL . min-1, the temperature of drift tube was 55 ℃ with Nitrogen as developing solvent. The linear calibration curve was obtained in the range of 0. 377-1. 844 μg with a linear correlation coefficient(r) of 0. 999 5. The RSD is 0.22% , and the add mark recovery was 96.78%. This method is simple, high sensitivity and good precision,it is suitable for determation D-pinitol in Lespedeza cuneata.
出处
《中国实验方剂学杂志》
CAS
北大核心
2011年第5期80-82,共3页
Chinese Journal of Experimental Traditional Medical Formulae
基金
安徽省国际合作项目(2009GH027)