高速逆流色谱-UPLC-Q-TOF-MS/MS法分离制备延胡索中脱氢紫堇碱和海罂粟碱

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。

Isolation and identification of dehydrocorydaline and glaucine from Corydalis Rhizoma by using high-speed counter-current chromatography and UPLC-Q-TOF-MS/MS

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 mL/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-of-flight 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.