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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 rapidly separate dehydrate corydaline and papaverine from Corydalis yanhusuo extract by high-speed countercurrent chromatography (HSCCC). Methods The mixed solvent of chloroform-n-butanol-methanol-water (4:1:2:5) was used as the two-phase solvent system. The rotation speed was 800 r / min and the volume flow rate was 10.0 m L / min. 30 min; reverse rotation speed of 800 r / min, volume flow 10.0 m L / min, elution time 30 min, detection wavelength 282 nm, 1 injection volume 50 mg; HPLC-UV analysis of the purity of the target product; The structure of the target product was identified by high performance liquid chromatography-tandem quadrupole time-of-flight mass spectrometry (UPLC-Q-TOF-MS / MS) Results Two kinds of monomers, 7.1 mg and 3.4 mg respectively, were obtained in yields of 81.43% and 91.11%, respectively, and their mass fractions were 98.9% and 94.3%, respectively. HPLC, UV and UPLC-Q-TOF MS / MS identification, respectively, dehydration corydalis and sea papaverine. Conclusion The method is rapid and simple and can be used as a method for the separation of corydaline and papaverine in Corydalis yanhusuo.