pH区带逆流色谱分离制备金果榄中的巴马汀及药根碱
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摘要
采用一种高效的pH区带逆流色谱方法分离制备金果榄中的巴马汀和药根碱,以氯仿-甲醇-水(4∶3∶2)为溶剂系统,在上相中加入20 mmol/L的HCl作为固定相,在下相中加入10 mmol/L三乙胺作为流动相,流速为2.0 mL/min,仪器转速为850 r/min。经一次pH区带逆流色谱分离,从2 g粗提物中得到512 mg巴马汀和421 mg药根碱。经高效液相色谱(HPLC)分析,其纯度均大于95%,采用MS,~1H NMR和~(13)C NMR对其化学结构进行确定。该方法具有简便、快捷、重现性好、上样量大等特点,可快速高效地分离制备金果榄中的巴马汀和药根碱。
An efficient method was developed for the preparative separation of palmatine and jatrorrhizine from Tinospora capillipes Gagnep. by pH- zone-refined counter-current chromatography( CCC).The two-phase solvent system of chloroform- methanol- water( 4 ∶ 3 ∶ 2) was selected,in which hydrochloric acid( 20 mmol / L) was added into the upper aqueous phase as the stationary phase,and triethylamine( 10 mmol / L) was added to the lower orgnic phase as the mobile phase. The apparatus was rotated at a speed of 850 r / min,while the mobile phase was pumped into the column at 2. 0 mL /min. From 2 g of crude extract,512 mg palmatine and 421 mg jatrorrhizine with purities of 95. 1%and 95. 3% were obtained. The chemical identification of the isolated compounds was carried out by electrospray ionization- mass spectrometry( ESI- MS),~1H NMR and~(13)C NMR. The introduced method is a rapid and efficient approach for the preparative separation of palmatine and jatrorrhizine in tinospora capillipes gagnep.
An efficient method was developed for the preparative separation of palmatine and jatrorrhizine from Tinospora capillipes Gagnep. by pH- zone-refined counter-current chromatography( CCC).The two-phase solvent system of chloroform- methanol- water( 4 ∶ 3 ∶ 2) was selected,in which hydrochloric acid( 20 mmol / L) was added into the upper aqueous phase as the stationary phase,and triethylamine( 10 mmol / L) was added to the lower orgnic phase as the mobile phase. The apparatus was rotated at a speed of 850 r / min,while the mobile phase was pumped into the column at 2. 0 mL /min. From 2 g of crude extract,512 mg palmatine and 421 mg jatrorrhizine with purities of 95. 1%and 95. 3% were obtained. The chemical identification of the isolated compounds was carried out by electrospray ionization- mass spectrometry( ESI- MS),~1H NMR and~(13)C NMR. The introduced method is a rapid and efficient approach for the preparative separation of palmatine and jatrorrhizine in tinospora capillipes gagnep.
引文
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[13]Wang Z M,Gao H M,Fu X T.China J.Chin.Mater.Med.(王智民,高慧敏,付雪涛.中国中药杂志),2006,31(23):1925-1928.
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[16]Jung H A,Yoon N Y,Bae H J,Min B S,Choi J S.Arch.Pharm.Res.,2008,31(11):1405-1412.