CN105384737B - 一种从吐根中提取精制生物碱的方法 - Google Patents
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- 244000284152 Carapichea ipecacuanha Species 0.000 title claims abstract description 39
- 239000009471 Ipecac Substances 0.000 title claims abstract description 38
- 229940029408 ipecac Drugs 0.000 title claims abstract description 38
- 238000000034 method Methods 0.000 title claims abstract description 29
- 229930013930 alkaloid Natural products 0.000 title claims abstract description 21
- 150000003797 alkaloid derivatives Chemical class 0.000 title claims abstract description 19
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- 238000006460 hydrolysis reaction Methods 0.000 title claims abstract description 15
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims abstract description 180
- 239000000243 solution Substances 0.000 claims abstract description 152
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 98
- 230000001476 alcoholic effect Effects 0.000 claims abstract description 30
- 239000000284 extract Substances 0.000 claims abstract description 27
- 239000000945 filler Substances 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 21
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- 230000002378 acidificating effect Effects 0.000 claims abstract description 20
- 239000006210 lotion Substances 0.000 claims abstract description 16
- 239000012071 phase Substances 0.000 claims abstract description 16
- 239000012141 concentrate Substances 0.000 claims abstract description 14
- 238000002347 injection Methods 0.000 claims abstract description 14
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- QISXROCIXKXUPS-OWVLCBNUSA-N Ipecoside Chemical compound O([C@@H]1OC=C([C@H]([C@H]1C=C)C[C@@H]1C2=CC(O)=C(O)C=C2CCN1C(C)=O)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O QISXROCIXKXUPS-OWVLCBNUSA-N 0.000 claims description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 26
- APCJEUAHYFIVKA-UHFFFAOYSA-N 5-trimethylsilylthiophene-2-carboxylic acid Chemical compound C[Si](C)(C)C1=CC=C(C(O)=O)S1 APCJEUAHYFIVKA-UHFFFAOYSA-N 0.000 claims description 24
- 239000011347 resin Substances 0.000 claims description 21
- 229920005989 resin Polymers 0.000 claims description 21
- HUEYSSLYFJVUIS-MRFSYGAJSA-N (2s,3r,11bs)-2-[[(1r)-6,7-dimethoxy-1,2,3,4-tetrahydroisoquinolin-1-yl]methyl]-3-ethyl-9,10-dimethoxy-2,3,4,6,7,11b-hexahydro-1h-benzo[a]quinolizine;hydron;chloride Chemical compound Cl.N1CCC2=CC(OC)=C(OC)C=C2[C@H]1C[C@H]1C[C@H]2C3=CC(OC)=C(OC)C=C3CCN2C[C@@H]1CC HUEYSSLYFJVUIS-MRFSYGAJSA-N 0.000 claims description 20
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- DTGZHCFJNDAHEN-OZEXIGSWSA-N cephaeline Chemical compound N1CCC2=CC(O)=C(OC)C=C2[C@H]1C[C@H]1C[C@H]2C3=CC(OC)=C(OC)C=C3CCN2C[C@@H]1CC DTGZHCFJNDAHEN-OZEXIGSWSA-N 0.000 claims description 8
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
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- QISXROCIXKXUPS-UHFFFAOYSA-N ipecoside Natural products C=CC1C(CC2C3=CC(O)=C(O)C=C3CCN2C(C)=O)C(C(=O)OC)=COC1OC1OC(CO)C(O)C(O)C1O QISXROCIXKXUPS-UHFFFAOYSA-N 0.000 description 1
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Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D455/00—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine
- C07D455/03—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing quinolizine ring systems directly condensed with at least one six-membered carbocyclic ring, e.g. protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine
- C07D455/04—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing quinolizine ring systems directly condensed with at least one six-membered carbocyclic ring, e.g. protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing a quinolizine ring system condensed with only one six-membered carbocyclic ring, e.g. julolidine
- C07D455/06—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing quinolizine ring systems directly condensed with at least one six-membered carbocyclic ring, e.g. protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing a quinolizine ring system condensed with only one six-membered carbocyclic ring, e.g. julolidine containing benzo [a] quinolizine ring systems
- C07D455/08—Heterocyclic compounds containing quinolizine ring systems, e.g. emetine alkaloids, protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing quinolizine ring systems directly condensed with at least one six-membered carbocyclic ring, e.g. protoberberine; Alkylenedioxy derivatives of dibenzo [a, g] quinolizines, e.g. berberine containing a quinolizine ring system condensed with only one six-membered carbocyclic ring, e.g. julolidine containing benzo [a] quinolizine ring systems having an isoquinolyl-1, a substituted isoquinolyl-1 or an alkylenedioxyisoquinolyl-1 radical linked through only one carbon atom, attached in position 2, e.g. emetine
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- A61K36/18—Magnoliophyta (angiosperms)
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- A61K31/47—Quinolines; Isoquinolines
- A61K31/4738—Quinolines; Isoquinolines ortho- or peri-condensed with heterocyclic ring systems
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
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- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
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Abstract
本发明公开一种从吐根中提取精制生物碱的方法,包括以下步骤:(1)提取浓缩:取吐根药材,粉碎,加入酸性甲醇溶液或酸性乙醇溶液进行提取,得提取液A,减压浓缩,得浓缩液B;(2)分离富集:上反相聚合填料J进行吸附,吸附完成后进行解析,先用水洗,收集水洗液C;再用醇溶液E洗脱,收集解析液D;(3)纯化:将水洗液C注入制备型高效液相进行分离纯化,收集溶液G;将解析液D注入制备型高效液相进行分离纯化,分别收集溶液H、溶液I;(4)富集干燥:将溶液G、溶液H、溶液I浓缩后,分别上反相聚合填料K进行吸附,吸附完成后,分别用醇溶液F洗脱,将洗脱后得到的洗脱液减压浓缩至干,真空干燥,即得,产品纯度高,收率高。
Description
技术领域
本发明涉及中药成分提取技术领域,具体涉及一种从吐根中提取精制生物碱的方法。
背景技术
吐根为茜草科植物Cephaelisipecacuanha(Brot.)A.Rich或Cephaelisacuminate Kar sten的干燥根茎,是巴西、哥斯达黎加或印度进口药材,在美国药典、日本药典及欧洲药典均有收载。现代药理学研究表明,吐根具有止咳化痰、催吐、抗阿米巴病等功效;有研究表明其主要药理活性成分为生物碱类化学成分,其中以吐根碱和吐根酚碱为主,两者占总生物碱的90%以上,由于吐根碱和吐根酚碱为游离态并不稳定,临床上多采用其盐酸盐进行治疗,其中盐酸吐根碱多用于治疗急性阿米巴病,而盐酸吐根酚碱则主要用于催吐和祛痰。吐根总生物碱中还有一种英文名为AIDS031406的生物碱,其CAS号为15401-60-2,其化学式为C27H35NO12,暂无中文名,其国内外的研究较少,目前只有用于实验室含量测定、对照试验、药理试验的市售产品,商品名为Ipecoside。
虽然吐根中各生物碱之间,如吐根碱和吐根酚碱的结构相近,但是其在人体内的吸收、分布、代谢和***是有很大差异的,各生物碱之间在药理上也是有一定差异的,为了更安全准确的用药,对于吐根中各生物碱的分离纯化精制是非常有必要的。然而吐根为进口药材,国内对其研究甚少,也缺乏相应的提取分离精制方法的文献,且国外文献中,对吐根中的吐根碱、吐根酚碱以及AIDS031406的提取分离方法也研究较少。CN102633793A的专利公开了从吐根中提取分离盐酸吐根碱和盐酸吐根酚碱的一种制备方法,采用超声提取、浓缩、萃取、分离纯化、冷冻干燥的步骤进行,得到的盐酸吐根碱和盐酸吐根酚碱的纯度超过98%,然而该制备方法是一种半制备方法,所用的试剂及设备都是实验室分析用的,其收率较小,产量低,只停留在实验室研究阶段,并不能实现工业化生产;同时萃取过程采用了***试剂,***是极易挥发的至麻醉试剂,使用及用量是严格控制的,根本就无法应用于生产。
发明内容
有鉴于此,本申请提供一种从吐根中提取精制生物碱的方法,所述方法能将吐根中的吐根碱、吐根酚碱以及AIDS031406以盐酸盐的形式提取分离出来,其中盐酸吐根碱的纯度达到98.5%以上,盐酸吐根酚碱的纯度达到98.5%以上,AIDS031406的纯度达到99%,总收率达到80%以上,产量高,适合于工业化生产,其方法简单,纯度较高,过程中除甲醇或乙醇外,不涉及其他有机溶剂,绿色环保。
为解决以上技术问题,本发明提供的技术方案是一种从吐根中提取精制生物碱的方法,所述方法包括以下步骤:
(1)提取浓缩:取吐根药材,粉碎,加入酸性甲醇溶液或酸性乙醇溶液进行提取,得提取液A,将提取液A进行减压浓缩,得浓缩液B;加入酸性甲醇溶液或酸性乙醇溶液的目的是将吐根中的吐根碱、吐根酚碱以及AIDS031406转化为稳定的盐酸盐形式;
(2)分离富集:取浓缩液B,上反相聚合填料J进行吸附,吸附完成后进行解析,先用水洗,收集水洗液C;再用醇溶液E洗脱,收集解析液D;其中水洗液C中为盐酸吐根酚碱,解析液D中为盐酸吐根碱和AIDS031406;
(3)纯化:将水洗液C注入制备型高效液相进行分离纯化,根据盐酸吐根酚碱的检测图谱相应谱带收集溶液G;将解析液D注入制备型高效液相进行分离纯化,根据盐酸吐根碱、AIDS031406的检测图谱相应谱带,分别收集溶液H、溶液I;通过制备型高效液相色谱,直接得到含有三种成分的纯品溶液,提高收率;
(4)富集干燥:将溶液G、溶液H、溶液I浓缩后,分别上反相聚合填料K进行吸附,吸附完成后,分别用醇溶液F洗脱,将洗脱后得到的洗脱液减压浓缩至干,再进行真空干燥,即得盐酸吐根酚碱纯品、盐酸吐根碱纯品、AIDS031406纯品。
优选的,步骤(1)中,所述酸性甲醇溶液或酸性乙醇溶液中,含有体积百分比为0.05%的盐酸,以及体积百分比为70—90%的甲醇或乙醇。
更为优选的,所述酸性甲醇溶液或酸性乙醇溶液中,甲醇或乙醇的体积百分比为80%。
优选的,步骤(1)中,提取液A减压浓缩的温度不高于65℃。
优选的,步骤(2)中,所述反相聚合填料J为任意一种选自AB-8型大孔吸附树脂、D101型大孔吸附树脂、XAD-16N填料、MCIGEL聚合填料、YMC填料、NM100-反相聚合物色谱填料。
更为优选的,步骤(2)中,所述反相聚合填料J为任意一种选自AB-8型大孔吸附树脂、D101型大孔树脂、NM100-反相聚合物色谱填料。
优选的,步骤(2)中,所述醇溶液E为甲醇溶液或乙醇溶液,所述醇溶液E中甲醇或乙醇的体积百分比为30—80%。
优选的,步骤(4)中,所述反相聚合填料K为AB-8型大孔吸附树脂。
优选的,步骤(4)中,所述醇溶液F为甲醇溶液或乙醇溶液,所述醇溶液F中甲醇或乙醇的体积百分比为80—100%。
优选的,步骤(4)中,所述减压浓缩的温度不高于55℃,所述真空干燥的温度为40—50℃。
本申请技术方案中的AB-8型大孔吸附树脂、D101型大孔吸附树脂、XAD-16N填料、MCI GEL聚合填料、YMC填料、NM100-反相聚合物色谱填料均为市售产品。
本申请与现有技术相比,其详细说明如下:本申请技术方案提供了从吐根中提取精制生物碱的方法,包括提取浓缩、分离富集、纯化、富集干燥的操作步骤,其中提取浓缩步骤中采用酸性甲醇溶液或酸性乙醇溶液进行提取,将吐根中的吐根碱、吐根酚碱以及AIDS031406转化为稳定的盐酸盐形式,有利于后续步骤的进行,同时提高产品纯度;在分离富集步骤中,采用反相聚合填料进行富集,将盐酸吐根酚碱、盐酸吐根碱与AIDS031406分离开来,其中水洗液C中为盐酸吐根酚碱,解析液D中为盐酸吐根碱和AIDS031406,此外避免了除甲醇或乙醇外其他有机溶剂的使用;在纯化步骤中,通过制备型高效液相色谱,直接得到含有三种成分的纯品溶液,提高收率;在富集干燥过程中,通过再一次富集,将纯品溶液由溶液形式转化为固体形式,经真空干燥后得到分离后的盐酸吐根酚碱纯品、盐酸吐根碱纯品、AIDS031406纯品。
经实验验证,所述方法中,盐酸吐根碱的纯度能达到98.5%以上,盐酸吐根酚碱的纯度能达到98.5%以上,AIDS031406的纯度能达到99%,其总收率达到80—90%,相比于现有技术中,纯度达到95%,收率仅为30%,本申请技术方案得到的成分纯度较高,收率上具有明显的优势,且方法简单,过程中除甲醇或乙醇外,不涉及其他有机溶剂,绿色环保。所述方法可用于标准品的精制制备,也可以用于工业化的生产,质量稳定可控,具有很好的应用前景。
具体实施方式
为了使本领域的技术人员更好地理解本发明的技术方案,下面结合具体实施例对本发明作进一步的详细说明。
实施例一
本实施例所述的从吐根中提取精制生物碱的方法,包括以下步骤:
(1)提取浓缩:取吐根药材,吐根药材产自哥斯达黎加,粉碎后,加入酸性甲醇溶液或酸性乙醇溶液进行提取,提取6次,合并得提取液A,将提取液A在60℃下减压浓缩,得浓缩液B;
(2)分离富集:取浓缩液B,上D101型大孔吸附树脂进行吸附,吸附完成后进行解析,先用水洗,收集水洗液C;再用浓度为45—60%的醇溶液E洗脱,收集解析液D,所述醇溶液E为甲醇溶液;
(3)分离纯化:将水洗液C注入制备型高效液相进行分离纯化,根据盐酸吐根酚碱的检测图谱相应谱带收集溶液G;将解析液D注入制备型高效液相进行分离纯化,根据盐酸吐根碱、AIDS031406的检测图谱相应谱带,分别收集溶液H、溶液I;
(4)富集干燥:将溶液G、溶液H、溶液I浓缩后,分别上AB-8型大孔吸附树脂进行吸附,吸附完成后,分别用浓度为95—100%的醇溶液F洗脱,所述醇溶液F为甲醇或乙醇溶液,将洗脱后得到的洗脱液在50℃下减压浓缩至干,再在45℃下真空干燥,即得盐酸吐根酚碱纯品、盐酸吐根碱纯品、AIDS031406纯品。
其中,所述步骤(1)中,根据酸性甲醇溶液或酸性乙醇溶液中甲醇或乙醇的体积百分比进行分组编号,其中1组为酸性甲醇溶液,甲醇的体积百分比为70%,2组为酸性甲醇溶液,甲醇的体积百分比为80%,3组为酸性甲醇溶液,甲醇的体积百分比为90%,4组为酸性乙醇溶液,乙醇的体积百分比为70%,5组为酸性乙醇溶液,乙醇的体积百分比为80%,6组为酸性乙醇溶液,乙醇的体积百分比为90%,上述各组中,其酸性均由体积百分比为0.05%的盐酸提供,通过HPLC分别检测每组方法中,所得盐酸吐根酚碱纯品、盐酸吐根碱纯品以及AIDS031406纯品的纯度,总生物碱的收率,分组检测结果见表1。
表1实施例一分组检测结果
从以上数据可以看出,上表中1—6组,其各组分纯度较高,均能达到98%以上,在高纯度的同时,且能达到至少80%的收率,其中第2组酸性甲醇溶液,甲醇的体积百分比为80%,其效果最好,为本申请的优选方案。
实施例二
本实施例所述的从吐根中提取精制生物碱的方法,包括以下步骤:
(1)提取浓缩:取吐根药材,吐根药材产自哥斯达黎加,粉碎后,加入酸性甲醇溶液进行提取,其中酸性甲醇溶液中,含有体积百分比为0.05%的盐酸,以及体积百分比为80%的甲醇,提取6次,合并得提取液A,将提取液A在60℃下减压浓缩,得浓缩液B;
(2)分离富集:取浓缩液B,上反相聚合填料J进行吸附,吸附完成后进行解析,先用水洗,收集水洗液C;再用浓度为45—60%的醇溶液E洗脱,收集解析液D,所述醇溶液E为甲醇或乙醇溶液;
(3)分离纯化:将水洗液C注入制备型高效液相进行分离纯化,根据盐酸吐根酚碱的检测图谱相应谱带收集溶液G;将解析液D注入制备型高效液相进行分离纯化,根据盐酸吐根碱、AIDS031406的检测图谱相应谱带,分别收集溶液H、溶液I;
(4)富集干燥:将溶液G、溶液H、溶液I浓缩后,分别上AB-8型大孔吸附树脂进行吸附,吸附完成后,分别用浓度为95—100%的醇溶液F洗脱,所述醇溶液F为甲醇或乙醇溶液,将洗脱后得到的洗脱液在50℃下减压浓缩至干,再在45℃下真空干燥,即得盐酸吐根酚碱纯品、盐酸吐根碱纯品、AIDS031406纯品。
其中,所述步骤(2)中,根据反相聚合填料J的选用不同进行分组编号,其中a组采用的是AB-8型大孔吸附树脂,b组采用的是D101型大孔吸附树脂,c组采用的是XAD-16N填料,d组采用的是MCIGEL聚合填料,e组采用的是YMC填料,f组采用的是NM100-反相聚合物色谱填料。通过HPLC分别检测每组方法中,所得盐酸吐根酚碱纯品、盐酸吐根碱纯品以及AIDS031406纯品的纯度,总生物碱的收率,分组检测结果见表2。
表2实施例二分组检测结果
从以上数据可以看出,a、b、f组采用的填料得到的纯度和收率数据均较好,因此,采用AB-8型大孔吸附树脂、D101型大孔树脂、NM100-反相聚合物色谱填料进行分离富集为本申请优选方案。
实施例三
本实施例所述的从吐根中提取精制生物碱的方法,包括以下步骤:
(1)提取浓缩:取吐根药材,吐根药材产自哥斯达黎加,粉碎后,加入酸性甲醇溶液进行提取,其中酸性甲醇溶液中,含有体积百分比为0.05%的盐酸,以及体积百分比为80%的甲醇,合并得提取液A,将提取液A在60℃下减压浓缩,得浓缩液B;
(2)分离富集:取浓缩液B,上AB-8型大孔吸附树脂进行吸附,吸附完成后进行解析,先用水洗,收集水洗液C;再用醇溶液E洗脱,收集解析液D;
(3)分离纯化:将水洗液C注入制备型高效液相进行分离纯化,根据盐酸吐根酚碱的检测图谱相应谱带收集溶液G;将解析液D注入制备型高效液相进行分离纯化,根据盐酸吐根碱、AIDS031406的检测图谱相应谱带,分别收集溶液H、溶液I;
(4)富集干燥:将溶液G、溶液H、溶液I浓缩后,分别上AB-8型大孔吸附树脂进行吸附,吸附完成后,分别用浓度为95—100%的醇溶液F洗脱,所述醇溶液F为甲醇或乙醇溶液,将洗脱后得到的洗脱液在50℃下减压浓缩至干,再在45℃下真空干燥,即得盐酸吐根酚碱纯品、盐酸吐根碱纯品、AIDS031406纯品。
其中,所述步骤(2)中,根据醇溶液E的醇种类和体积百分比不同进行分组编号,其中g组为甲醇溶液,体积百分比为30—45%,h组为甲醇溶液,体积百分比为45—60%,i组为甲醇溶液,体积百分比为60—70%,j组为甲醇溶液,体积百分比为70—80%,k组为乙醇溶液,体积百分比为30—45%,l组为乙醇溶液,体积百分比为45—60%,m组为乙醇溶液,体积百分比为60—70%,n组为乙醇溶液,体积百分比为70—80%。通过HPLC分别检测每组方法中,所得盐酸吐根酚碱纯品、盐酸吐根碱纯品以及AIDS031406纯品的纯度,总生物碱的收率,分组检测结果见表3。
表3实施例三分组检测结果
从以上数据可以看出,采用甲醇或采用乙醇得到的纯度和收率均较高,其中,h和l组的数据更好,即甲醇或乙醇的体积比为45—60%时,效果最好,为本申请的优选技术方案。
实施例四
本实施例所述的从吐根中提取精制生物碱的方法,包括以下步骤:
(1)提取浓缩:取吐根药材,吐根药材产自哥斯达黎加,粉碎后,加入酸性甲醇溶液进行提取,其中酸性甲醇溶液中,含有体积百分比为0.05%的盐酸,以及体积百分比为80%的甲醇,提取6次,合并得提取液A,将提取液A在60℃下减压浓缩,得浓缩液B;
(2)分离富集:取浓缩液B,上NM100-反相聚合物色谱填料进行吸附,吸附完成后进行解析,先用水洗,收集水洗液C;再用浓度为45—60%的醇溶液E洗脱,收集解析液D,所述醇溶液E为甲醇溶液;
(3)分离纯化:将水洗液C注入制备型高效液相进行分离纯化,根据盐酸吐根酚碱的检测图谱相应谱带收集溶液G;将解析液D注入制备型高效液相进行分离纯化,根据盐酸吐根碱、AIDS031406的检测图谱相应谱带,分别收集溶液H、溶液I;
(4)富集干燥:将溶液G、溶液H、溶液I浓缩后,分别上AB-8型大孔吸附树脂进行吸附,吸附完成后,分别用醇溶液F洗脱,将洗脱后得到的洗脱液在50℃下减压浓缩至干,再在45℃下真空干燥,即得盐酸吐根酚碱纯品、盐酸吐根碱纯品、AIDS031406纯品。
其中,所述步骤(4)中,根据醇溶液F的醇种类和体积百分比不同进行分组编号,其中Ⅰ组为甲醇溶液,体积百分比为80—85%,Ⅱ组为甲醇溶液,体积百分比为85—90%,Ⅲ组为甲醇溶液,体积百分比为90—95%,Ⅳ组为甲醇溶液,体积百分比为95—100%,Ⅴ组为乙醇溶液,体积百分比为80—85%,Ⅵ组为乙醇溶液,体积百分比为85—90%,Ⅶ组为乙醇溶液,体积百分比为90—95%,Ⅷ组为乙醇溶液,体积百分比为95—100%。通过HPLC分别检测每组方法中,所得盐酸吐根酚碱纯品、盐酸吐根碱纯品以及AIDS031406纯品的纯度,总生物碱的收率,分组检测结果见表4。
表4实施例四分组检测结果
从以上试验数据可以看出,Ⅳ组和Ⅷ组中的各组分的纯度和收率均较高,因此采用体积比为95—100%的甲醇或乙醇,其效果最好,收率最高,为本申请的优选技术方案。
以上仅是本发明的优选实施方式,应当指出的是,上述优选实施方式不应视为对本发明的限制,本发明的保护范围应当以权利要求所限定的范围为准。对于本技术领域的普通技术人员来说,在不脱离本发明的精神和范围内,还可以做出若干改进和润饰,这些改进和润饰也应视为本发明的保护范围。
Claims (5)
1.一种从吐根中提取精制生物碱的方法,其特征在于:所述方法包括以下步骤:
(1)提取浓缩:取吐根药材,粉碎,加入酸性甲醇溶液或酸性乙醇溶液进行提取,得提取液A,将提取液A进行减压浓缩,得浓缩液B;所述酸性甲醇溶液或酸性乙醇溶液中,含有体积百分比为0.05%的盐酸,以及体积百分比为70—90%的甲醇或乙醇;
(2)分离富集:取浓缩液B,上反相聚合填料J进行吸附,吸附完成后进行解析,先用水洗,收集水洗液C;再用醇溶液E洗脱,收集解析液D;所述反相聚合填料J为任意一种选自AB-8型大孔吸附树脂、D101型大孔吸附树脂、XAD-16N填料、MCI GEL聚合填料、YMC填料、NM100-反相聚合物色谱填料;所述醇溶液E为甲醇溶液或乙醇溶液,所述醇溶液E中甲醇或乙醇的体积百分比为30—80%;
(3)纯化:将水洗液C注入制备型高效液相进行分离纯化,根据盐酸吐根酚碱的检测图谱相应谱带收集溶液G;将解析液D注入制备型高效液相进行分离纯化,根据盐酸吐根碱、AIDS031406的检测图谱相应谱带,分别收集溶液H、溶液I;
(4)富集干燥:将溶液G、溶液H、溶液I浓缩后,分别上反相聚合填料K进行吸附,吸附完成后,分别用醇溶液F洗脱,将洗脱后得到的洗脱液减压浓缩至干,再进行真空干燥,即得盐酸吐根酚碱纯品、盐酸吐根碱纯品、AIDS031406纯品;所述反相聚合填料K为AB-8型大孔吸附树脂;所述醇溶液F为甲醇溶液或乙醇溶液,所述醇溶液F中甲醇或乙醇的体积百分比为80—100%。
2.根据权利要求1所述的一种从吐根中提取精制生物碱的方法,其特征在于:所述酸性甲醇溶液或酸性乙醇溶液中,甲醇或乙醇的体积百分比为80%。
3.根据权利要求1所述的一种从吐根中提取精制生物碱的方法,其特征在于:步骤(1)中,提取液A减压浓缩的温度不高于65℃。
4.根据权利要求1所述的一种从吐根中提取精制生物碱的方法,其特征在于:步骤(2)中,所述反相聚合填料J为任意一种选自AB-8型大孔吸附树脂、D101型大孔树脂、NM100-反相聚合物色谱填料。
5.根据权利要求1所述的一种从吐根中提取精制生物碱的方法,其特征在于:步骤(4)中,所述减压浓缩的温度不高于55℃,所述真空干燥的温度为40—50℃。
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