CN110372591A - 一种秃疮花中紫堇碱和异紫堇碱的提取分离方法 - Google Patents
一种秃疮花中紫堇碱和异紫堇碱的提取分离方法 Download PDFInfo
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- C07D221/02—Heterocyclic compounds containing six-membered rings having one nitrogen atom as the only ring hetero atom, not provided for by groups C07D211/00 - C07D219/00 condensed with carbocyclic rings or ring systems
- C07D221/04—Ortho- or peri-condensed ring systems
- C07D221/18—Ring systems of four or more rings
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D471/00—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00
- C07D471/02—Heterocyclic compounds containing nitrogen atoms as the only ring hetero atoms in the condensed system, at least one ring being a six-membered ring with one nitrogen atom, not provided for by groups C07D451/00 - C07D463/00 in which the condensed system contains two hetero rings
- C07D471/04—Ortho-condensed systems
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Abstract
本发明公开了一种秃疮花中紫堇碱和异紫堇碱的提取分离方法,采用95%乙醇超声提取法,防止高温改变物质的结构和性质,简化提取工艺,减少环境污染,纯化率高。本发明的紫堇碱和异紫堇碱的提取分离方法,分离后分别得到紫堇碱和异紫堇碱,而不是紫堇碱和异紫堇碱的混合物,纯化率高。
Description
技术领域
本发明涉及植物提取技术领域,尤其涉及一种秃疮花中紫堇碱和异紫堇碱的提取分离方法。
背景技术
秃疮花(Dicranostigma leptopodum),又名红茂草、秃子花,为罂粟科秃疮花属植物,主要分布于我国秦岭以北,甘肃和陕西黄土高原地区,全草有清热解毒、消肿止痛、杀虫等功效(柳军玺,秃疮花生物碱类化学成分研究,中草药,2011,8,1505-1508.)。紫金龙(Dactylicapnos scandens(D.Don))Hutch,又名串枝莲、碗豆七等,为罂粟科紫金龙属植物,主要分布于云南、四川、广西、西藏等地,其根入药有镇痛、止血、消炎、降压之功效,可治疗多种疼痛,是我国云南白族传统习用中草药(钱金栿,白族草药紫金龙成分的研究,西北药学杂志,2000,15,57-58.)。广西地不容(Stephania kwangsiensis H.S.Lo)为防己科千金藤属植物,主要分布于广西中部至西南部、贵州南部及云南文山地区;块根主治感冒头痛、胃痛、咽喉痛、痢疾、疮痈肿痛、外伤疼痛。
紫堇碱异名为延胡索碱或延胡索甲素,英文名为Corydaline或corydaline,分子式为C22H27NO4,为季胺类生物碱,是罂粟科紫堇属植物延胡索(CorydalisyanhusuoW.T.Wang)块茎中的主要有效成分之一。现代药理学表明延胡索甲素不仅有镇痛、兴奋子宫、抗心律失常等作用,还可用于制备为戒毒药物。也有延胡索甲素在抗呼吸道病毒及治疗呼吸道病毒感染引起疾病的报道。
异紫堇碱(Isocorydine),也叫异紫堇啡碱,异紫堇定,异可利定,属阿朴菲型生物碱植物次生代谢产物,具有较好的药理活性,该化合物广泛分布于木兰科、防己科、大戟科、樟科、马钱科、番荔枝科、马兜铃科、小檗科、罂粟科、毛茛科、芸香科等多科植物中(赵奇志,阿朴菲类生物碱生物活性研究进展,天然产物研究与开发,2006,18,316-324.),异紫堇碱在秃疮花,紫金龙,广西地不容,山胡椒,小藤铃儿草,洋玉兰等植物中含量较高。1992年Ribar确定了异紫堇碱的化学结构(Ribar B,Structure of isocorydine,ActaCrystallogr C,1992,48,945-947.),对于异紫堇碱的药理活性已经有过很多研究,ChenZH等在1982年报道异紫堇碱对于内脏平滑肌的非特异解痉作用(Chen ZH,Spasmolyticeffect of isocorydine on isolated vascular strips,Acta PharmacolSin,1982,3,240-242.),2001年Jiang QS等人认为异紫堇碱有舒张血管的作用(Jiang QS,Relation ofvasodilative action of isocorydine to cyclic nucleotides,Chin JPharm Toxicol,2001,15,251-255.),2003年,国家药监局批准异可利定盐酸盐作为处方药(H53021977)用于胃、肠、胆、胰、子宫、血管痉挛所致的疼痛。
中国发明专利CN 104072418A提供了一种利用聚苯乙烯二乙烯基苯聚合制成的大孔树脂作为选择性吸附剂,从秃疮花、地不容、金钱吊乌龟及紫堇等植物提取物中选择吸附,分离纯化异紫堇碱的制备方法。但是该方法通过大孔树脂吸附柱洗脱除杂,工艺繁重复杂,且只能得到异紫堇碱,而浪费了紫堇碱。故有必要对秃疮花中紫堇碱和异紫堇碱的提取分离技术做进一步的研究。
发明内容
本发明提供了一种秃疮花中紫堇碱和异紫堇碱的提取分离纯化技术路线,采用乙醇超声提取法,防止高温改变物质的结构和性质,简化提取工艺,减少环境污染,纯化率高。
一种秃疮花中紫堇碱和异紫堇碱的提取分离方法,包括以下步骤:
A、秃疮花全草药材干燥粉碎,取其干粉,用乙醇溶液超声波提取3-4次,温度为42-48℃,每次45-75min,过滤,合并滤液,60-70℃减压回收溶剂,制得乙醇提取物;
B、充分混悬后,再依次用极性由小到大的不同溶剂萃取:首先用等量石油醚溶剂连续萃取3-4次,混合萃取液,并减压蒸馏除去石油醚溶剂,得石油醚萃取相浸膏;剩余水相,加入1.5-2.5%盐酸进行酸化,并调节至pH为1-2,然后用等量氯仿溶剂萃取3-4次,合并萃取液,并减压除去氯仿溶剂,得酸化氯仿相浸膏;
C、取酸化氯仿相浸膏,干法上样,硅胶柱层析,依次用洗脱剂CHCl3:CH3OH=10:1、9:1得到紫堇碱和异紫堇碱。
优选的,所述的步骤A中,所述的乙醇溶液为体积分数为95%的乙醇溶液。
优选的,所述的步骤A中,所述的乙醇溶液的质量为药材的4-6倍量,即在常压下固液比(g/mL)为1:(4-6)。
本发明的有益之处在于:本发明的秃疮花中紫堇碱和异紫堇碱的提取分离方法,采用95%乙醇超声提取法,防止高温改变物质的结构和性质,简化提取工艺,减少环境污染,纯化率高。本发明的紫堇碱和异紫堇碱的提取分离方法,分离后分别得到紫堇碱和异紫堇碱,而不是紫堇碱和异紫堇碱的混合物,纯化率高。
具体实施方式
实施例1:
一种秃疮花中紫堇碱和异紫堇碱的提取分离方法,包括以下步骤:
A、秃疮花全草药材干燥粉碎,取其干粉400g,用95%乙醇溶液2000mL超声波提取3次,温度为45℃,每次60min,过滤,合并滤液,65℃减压回收溶剂,制得乙醇提取物;
B、充分混悬后,再依次用极性由小到大的不同溶剂萃取:首先用等量石油醚溶剂连续萃取3次,混合萃取液,并减压蒸馏除去石油醚溶剂,得石油醚萃取相浸膏;剩余水相,加入2.0%盐酸进行酸化,并调节至pH为1.5,然后用等量氯仿溶剂萃取3次,合并萃取液,并减压除去氯仿溶剂,得酸化氯仿相浸膏;
C、取酸化氯仿相浸膏,干法上样,硅胶柱层析,依次用洗脱剂CHCl3:CH3OH=10:1、9:1得到紫堇碱和异紫堇碱。
所述的步骤A中,所述的乙醇溶液的质量为药材的5倍量,即在常压下固液比(g/mL)为1:5。
实施例2:
一种秃疮花中紫堇碱和异紫堇碱的提取分离方法,包括以下步骤:
A、秃疮花全草药材干燥粉碎,取其干粉400g,用95%乙醇溶液2000mL超声波提取3次,温度为48℃,每次45min,过滤,合并滤液,70℃减压回收溶剂,制得乙醇提取物;
B、充分混悬后,再依次用极性由小到大的不同溶剂萃取:首先用等量石油醚溶剂连续萃取3次,混合萃取液,并减压蒸馏除去石油醚溶剂,得石油醚萃取相浸膏;剩余水相,加入2.5%盐酸进行酸化,并调节至pH为1.0,然后用等量氯仿溶剂萃取4次,合并萃取液,并减压除去氯仿溶剂,得酸化氯仿相浸膏;
C、取酸化氯仿相浸膏,干法上样,硅胶柱层析,依次用洗脱剂CHCl3:CH3OH=10:1、9:1得到紫堇碱和异紫堇碱。
所述的步骤A中,所述的乙醇溶液的质量为药材的4倍量,即在常压下固液比(g/mL)为1:4。
实施例3:
一种秃疮花中紫堇碱和异紫堇碱的提取分离方法,包括以下步骤:
A、秃疮花全草药材干燥粉碎,取其干粉400g,用95%乙醇溶液2000mL超声波提取3-4次,温度为42℃,每次75min,过滤,合并滤液,60℃减压回收溶剂,制得乙醇提取物;
B、充分混悬后,再依次用极性由小到大的不同溶剂萃取:首先用等量石油醚溶剂连续萃取4次,混合萃取液,并减压蒸馏除去石油醚溶剂,得石油醚萃取相浸膏;剩余水相,加入1.5%盐酸进行酸化,并调节至pH为2.0,然后用等量氯仿溶剂萃取3次,合并萃取液,并减压除去氯仿溶剂,得酸化氯仿相浸膏;
C、取酸化氯仿相浸膏,干法上样,硅胶柱层析,依次用洗脱剂CHCl3:CH3OH=10:1、9:1得到紫堇碱和异紫堇碱。
所述的步骤A中,所述的乙醇溶液的质量为药材的6倍量,即在常压下固液比(g/mL)为1:6。
经检测,本发明实施例1中,异紫堇碱占酸化氯仿相的48.9%,紫堇碱占酸化氯仿相的19.7%,两者合计共占酸化氯仿相的68.6%,以前的工艺得到的是紫堇碱和异紫堇碱的混合物,没有进一步分离纯化,此结果已经通过1HNMR、13CNMR、DEPT以及HPLC检测二者积分面积和保留时间不同而加以鉴别确认。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (4)
1.一种秃疮花中紫堇碱和异紫堇碱的提取分离方法,其特征在于,包括以下步骤:
A、秃疮花全草药材干燥粉碎,取其干粉,用乙醇溶液超声波提取3-4次,温度为42-48℃,每次45-75min,过滤,合并滤液,60-70℃减压回收溶剂,制得乙醇提取物;
B、充分混悬后,再依次用极性由小到大的不同溶剂萃取:首先用等量石油醚溶剂连续萃取3-4次,混合萃取液,并减压蒸馏除去石油醚溶剂,得石油醚萃取相浸膏;剩余水相,加入1.5-2.5%盐酸进行酸化,并调节至pH为1-2,然后用等量氯仿溶剂萃取3-4次,合并萃取液,并减压除去氯仿溶剂,得酸化氯仿相浸膏;
C、取酸化氯仿相浸膏,干法上样,硅胶柱层析,依次用洗脱剂CHCl3:CH3OH=10:1、9:1得到紫堇碱和异紫堇碱。
2.如权利要求1所述的秃疮花中紫堇碱和异紫堇碱的提取分离方法,其特征在于,所述的步骤A中,所述的乙醇溶液为体积分数为95%的乙醇溶液。
3.如权利要求1所述的秃疮花中紫堇碱和异紫堇碱的提取分离方法,其特征在于,所述的步骤A中,所述的乙醇溶液的质量为药材的4-6倍量,即在常压下固液比(g/mL)为1:(4-6)。
4.如权利要求1所述的秃疮花中紫堇碱和异紫堇碱的提取分离方法,其特征在于,包括以下步骤:
A、秃疮花全草药材干燥粉碎,取其干粉,用95%乙醇溶液超声波提取3次,温度为45℃,每次60min,过滤,合并滤液,65℃减压回收溶剂,制得乙醇提取物;
B、充分混悬后,再依次用极性由小到大的不同溶剂萃取:首先用等量石油醚溶剂连续萃取3次,混合萃取液,并减压蒸馏除去石油醚溶剂,得石油醚萃取相浸膏;剩余水相,加入2.0%盐酸进行酸化,并调节至pH为1.5,然后用等量氯仿溶剂萃取3次,合并萃取液,并减压除去氯仿溶剂,得酸化氯仿相浸膏;
C、取酸化氯仿相浸膏,干法上样,硅胶柱层析,依次用洗脱剂CHCl3:CH3OH=10:1、9:1得到紫堇碱和异紫堇碱;
所述的步骤A中,所述的乙醇溶液的质量为药材的5倍量,即在常压下固液比(g/mL)为1:5。
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