CAJ | 학술논문

目的：分离纯化吴茱萸中的活性成分。方法应用pH区带逆流色谱，以氯仿-乙酸乙酯-甲醇-水（3：1：3：3，v/v）为两相溶剂体系，上相加入10 mmol/L盐酸作为固定相；下相加入5 mmol/L三乙胺作为流动相，转速850 r/min，流速2.0 mL/min，检测波长254 nm，所得馏分经HPLC检测，并经电喷雾电离（ESI）质谱和核磁共振谱（NMR）鉴定化合物的结构。结果从2 g吴茱萸粗提物中一次性分离得101 mg吴茱萸碱和304 mg去氢吴茱萸碱，其纯度为90.0%和93.1%。结论此法简便、快捷、重现性好、上样量大，适于制备性分离吴茱萸碱和去氢吴茱萸碱。
목적：분리순화오수유중적활성성분。방법응용pH구대역류색보，이록방-을산을지-갑순-수（3：1：3：3，v/v）위량상용제체계，상상가입10 mmol/L염산작위고정상；하상가입5 mmol/L삼을알작위류동상，전속850 r/min，류속2.0 mL/min，검측파장254 nm，소득류분경HPLC검측，병경전분무전리（ESI）질보화핵자공진보（NMR）감정화합물적결구。결과종2 g오수유조제물중일차성분리득101 mg오수유감화304 mg거경오수유감，기순도위90.0%화93.1%。결론차법간편、쾌첩、중현성호、상양량대，괄우제비성분리오수유감화거경오수유감。
Objective To separate and purify the active ingredients from Evodia rutaecarpa. Methods A pH zone countercurrent chromatography was used with chloroform-ethyl acetate-methanol-water (3:1:3:3, v/v) as a two-phase solvent system;the upper phase was used as the stationary phase by adding 10 mmol/L hydrochloric acid, the lower phase was used as the mobile phase by adding 5 mmol/L triethylamine, with the rotary speed of 850 r/min and a flow rate of 2.0 mL/min. The detection wavelength was 254 nm. The separated fractions were detected by HPLC, and the structures of the compounds were identified by ESI-MS and NMR. Results Evodiamine (101 mg) and dehydroevodiamine (304 mg) were isolated from 2 g crude extract of Evodia rutaecarpa, with the purity of 90.0%and 93.1%, respectively. Conclusion The method is simple, rapid, reproducible and of large loading capacity, and suitable for the preparative separation of evodiamine and dehydroevodiamine.