摘要
目的 :从苦地丁中制备紫堇灵和乙酰紫堇灵 ,并建立同时测定二者含量的反相高效液相色谱法。方法 :采用柱层析分离、制备 ,波谱方法及理化性质鉴定二化合物 ;用HPLC法进行含量测定 ,色谱柱为APEX ODS柱 ,流动相为甲醇 1 5mmol·L- 1 磷酸二氢钾 /磷酸氢二钾缓冲液 (pH 6 .70 ,70∶30 ) ,流速 0 .8mL·min- 1 ,检测波长2 89nm ,采用外标两点法定量。结果 :得到紫堇灵和乙酰紫堇灵的纯度在 99%以上 ;紫堇灵在 6 .9～ 1 1 0 .4mg·L- 1 ,乙酰紫堇灵在 8.7～ 1 39.5mg·L- 1 线性关系良好 ;RSD分别为 2 .1 % ,2 .7% ,回收率 97.3 % ,97.2 %。结论 :建立了紫堇灵和乙酰紫堇灵的制备方法 ;HPLC方法简单 ,易操作 。
Objective: To isolate and purify corynoline and acetylcorynoline from Corydalis bungeana and develop a reversed phase HPLC method of determining the two components in C. bungeana . Method: Alkaloids were isolated from the ethanolic extract with column gel chromatography, and identified on the basis of spectral analysis (UV, 1H NMR, 13 C NMR) and physicochemical properties. For quantitative analysis of the two components, samples were separated on an ODS column with mobile phase of methanol 15 mmol·L -1 potassium dihydrogen phosphate/potassium phosphate dibasic (pH 6.70,70∶30). The flow rate was 0.8 mL·min -1 , and the detection was set at 289 nm. Result: The purity was 99.5% and 99.1% for corynoline and acetylcorynoline respectively. The calibration curves were linear in the range of 6.9～110.4 mg·L -1 corynoline and 8.7～139.5 mg·L -1 acetylcorynoline. The RSD was 2.1% and 2.7%,and the average recovery was 97.3% and 97.2% respectively. Conclusion: The method of isolating and purifying corynoline and acetylcorynoline from Corydalis bungeana and the HPLC method of simultaneous determination of the two components have been developed. The HPLC method is simple, easy to perform and applicable to the content determination of corynoline and acetylcorynoline in C. bungeana of various origins.[
出处
《中国中药杂志》
CAS
CSCD
北大核心
2003年第4期346-349,共4页
China Journal of Chinese Materia Medica
