摘要
目的建立酸枣仁提取物薄层色谱鉴别方法及高效液相色谱-蒸发光散射检测法（HPLC-ELSD）同时测定酸枣仁皂苷A、B和斯皮诺素含量的方法。方法以水饱和正丁醇为展开剂,采用硅胶G板进行定性鉴别;采用HPLC-ELSD法进行定量测定,Kromasil C18色谱柱（200 mm×4.6 mm,5μm）;流动相为乙腈（A）-水（B）,梯度洗脱（0~15 min,20%A→40%A;15~22 min,40%A;22~24 min,40%A→80%A;24~30 min,80%A→100%A;30~40 min,100%A）;流速：1.0 m L·min-1;柱温：25℃,蒸发光散射检测器,漂移管温度：50℃,衰减6。结果酸枣仁提取物薄层色谱法鉴别效果良好。酸枣仁皂苷A、酸枣仁皂苷B和斯皮诺素的线性范围分别为0.105~1.68μg（r=0.9998）,0.0743~1.1885μg（r=0.9995）,0.2972~4.757μg（r=0.9992）;平均回收率分别为97.6%,99.9%,104.8%,RSD分别为：1.2%,1.9%和1.0%（n=6）。结论薄层色谱法简便,稳定;HPLC-ELSD法准确,具有良好的重复性和稳定性;适用于酸枣仁提取物的定性鉴别和定量测定。
Objective To establish thin layer chromatography（TLC）method for identifying the extract of Semen Ziziphi Spinosae,and to develop a method of high performance liquid chromatography- evaporative light scattering detector（HPLC-ELSD）for the simultaneous determination of jujuboside A,jujuboside B and spinosin in the extract of Semen Ziziphi Spinosae. Methods N-butanol saturated with water was used as solvent system and silica gel G was used as stationary phase for the identification of extract of Semen Ziziphi Spinosae. HPLC-ELSD method was adopted for the quantitative analysis. The analysis was performed on a Kromasil C18column（200 mm×4.6 mm,5 μm）with the mobile phase consisting of acetonitrile（A）-water（B）by gradient elution（0~15 min,20 %A→40 %A;15~22 min,40 %A;22~24 min,40 % A→80 % A;24~30 min,80 % A→100 % A;30~40 min,100 % A） at 25 ℃ with a flow rate of 1.0 m L·min^-1. The evaporative light scattering detector was set at 50 ℃,and the decay gradient was set at6. Results The TLC method was good for the identification of extract of Semen Ziziphi Spinosae. The linear range was0.105~1.68 μg（r=0.9998）for jujuboside A,0.0743~1.1885 μg（r=0.9995）for jujuboside B,and 0.2972~4.757μg（r=0.9992）for spinosin. The average recoveries（n=6） of three components were 97.6 %,99.9 % and 104.8 % and RSD was 1.2 %,1.9 % and 1.0 %,respectively. Conclusion The TLC method is rapid and stable. The HPLC-ELSD method is accurate and reproducible. The established methods are suitable for the identification and quantitative determination of the extract of Semen Ziziphi Spinosae.
出处
《中药新药与临床药理》
CAS
CSCD
北大核心
2015年第3期365-369,共5页
Traditional Chinese Drug Research and Clinical Pharmacology
基金
广东省科技计划项目(2011B031700063)
