摘要
目的采用高速逆流色谱(HSCCC)快速分离延胡索提取物中脱氢紫堇碱和海罂粟碱。方法以氯仿-正丁醇-甲醇-水(4∶1∶2∶5)混合溶剂作为两相溶剂体系,正转,转速为800 r/min,体积流量为10.0 m L/min,洗脱时间30 min;反转,转速为800 r/min,体积流量10.0 m L/min,洗脱时间30 min,检测波长282 nm,1次进样量50 mg;HPLC-UV法分析目标产物纯度;超高效液相色谱串联四级杆飞行时间质谱(UPLC-Q-TOF-MS/MS)法对目标产物进行结构鉴定。结果制备得到7.1 mg和3.4 mg 2种单体,收率分别为81.43%和91.11%,利用HPLC法测得其质量分数分别为98.9%和94.3%;经HPLC、紫外光谱和UPLC-Q-TOF-MS/MS鉴定,分别为脱氢紫堇碱和海罂粟碱。结论该方法快速、简便,可以作为对延胡索中脱氢紫堇碱和海罂粟碱的分离制备方法。
Objective To isolate dehydrocorydaline and glaucine by high-speed counter-current chromatography（HSCCC） from the extraction of Corydalis Rhizoma（CR）. Methods A mixture of chloroform-n-butanol-methanol-water（4∶1∶2∶5） was used as the two phase solvent system both in forward and reversal direction, with a flow rate of 10.0 m L/min and a rotary speed of 800 r/min eluting for 30 min. The detection wavelength was 282 nm and injection volume was 50 mg. The purity of the target product was analyzed by HPLC-UV and the structure was identified by ultra performance liquid chromatography-tandem quadrupole time-offlight mass spectrometry（UPLC-Q-TOF-MS/MS）. Results Under optimized conditions, 7.1 mg and 3.4 mg of two compounds were obtained and their yields were 81.43% and 91.11% respectively. Their purities were 98.9% and 94.3% detected by HPLC. dehydrocorydaline and glaucine were identifiled through HPLC, ultraviolet absorbance, and UPLC-Q-TOF-MS/MS. Conclusion The result indicate that HSCCC is a powerful technique for the purification of dehydrocorydaline and glaucine from CR.
出处
《中草药》
CAS
CSCD
北大核心
2016年第24期4351-4356,共6页
Chinese Traditional and Herbal Drugs
基金
国家自然基金资助项目(30870257)
成都市科技惠民技术研发项目(2015-HM01-00617-SF)
