CN111603500B - 一种决明子提取物及决明子综合开发利用的工艺技术 - Google Patents
一种决明子提取物及决明子综合开发利用的工艺技术 Download PDFInfo
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- 210000000582 semen Anatomy 0.000 title claims abstract description 28
- 239000000284 extract Substances 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 14
- 230000008569 process Effects 0.000 title claims abstract description 10
- 238000005516 engineering process Methods 0.000 title claims abstract description 9
- 244000037364 Cinnamomum aromaticum Species 0.000 claims abstract description 40
- 235000014489 Cinnamomum aromaticum Nutrition 0.000 claims abstract description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 35
- OMDQUFIYNPYJFM-XKDAHURESA-N (2r,3r,4s,5r,6s)-2-(hydroxymethyl)-6-[[(2r,3s,4r,5s,6r)-4,5,6-trihydroxy-3-[(2s,3s,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxyoxan-2-yl]methoxy]oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@@H]1OC[C@@H]1[C@@H](O[C@H]2[C@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)[C@H](O)[C@H](O)[C@H](O)O1 OMDQUFIYNPYJFM-XKDAHURESA-N 0.000 claims abstract description 32
- 229920000926 Galactomannan Polymers 0.000 claims abstract description 32
- 238000000605 extraction Methods 0.000 claims abstract description 16
- PYKYMHQGRFAEBM-UHFFFAOYSA-N anthraquinone Natural products CCC(=O)c1c(O)c2C(=O)C3C(C=CC=C3O)C(=O)c2cc1CC(=O)OC PYKYMHQGRFAEBM-UHFFFAOYSA-N 0.000 claims abstract description 15
- 150000004056 anthraquinones Chemical class 0.000 claims abstract description 15
- 239000008346 aqueous phase Substances 0.000 claims abstract description 9
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000000463 material Substances 0.000 claims abstract description 6
- RJRZRMYKFWYPNX-UHFFFAOYSA-N [NH4+].[NH4+].CCO.[O-]S([O-])(=O)=O Chemical compound [NH4+].[NH4+].CCO.[O-]S([O-])(=O)=O RJRZRMYKFWYPNX-UHFFFAOYSA-N 0.000 claims abstract description 3
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- 239000006228 supernatant Substances 0.000 claims description 14
- 238000001914 filtration Methods 0.000 claims description 13
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 12
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 12
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 8
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- 238000005119 centrifugation Methods 0.000 claims description 2
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 2
- 238000002386 leaching Methods 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000002893 slag Substances 0.000 claims description 2
- 238000009776 industrial production Methods 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 239000003960 organic solvent Substances 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 150000004676 glycans Chemical class 0.000 description 5
- 229920001282 polysaccharide Polymers 0.000 description 5
- 239000005017 polysaccharide Substances 0.000 description 5
- 239000003814 drug Substances 0.000 description 4
- 239000012535 impurity Substances 0.000 description 4
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 3
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- LQGUBLBATBMXHT-UHFFFAOYSA-N chrysophanol Chemical compound C1=CC=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O LQGUBLBATBMXHT-UHFFFAOYSA-N 0.000 description 2
- 235000013373 food additive Nutrition 0.000 description 2
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- 241000894006 Bacteria Species 0.000 description 1
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- VWDXGKUTGQJJHJ-UHFFFAOYSA-N Catenarin Natural products C1=C(O)C=C2C(=O)C3=C(O)C(C)=CC(O)=C3C(=O)C2=C1O VWDXGKUTGQJJHJ-UHFFFAOYSA-N 0.000 description 1
- 239000010282 Emodin Substances 0.000 description 1
- RBLJKYCRSCQLRP-UHFFFAOYSA-N Emodin-dianthron Natural products O=C1C2=CC(C)=CC(O)=C2C(=O)C2=C1CC(=O)C=C2O RBLJKYCRSCQLRP-UHFFFAOYSA-N 0.000 description 1
- 241000220485 Fabaceae Species 0.000 description 1
- YOOXNSPYGCZLAX-UHFFFAOYSA-N Helminthosporin Natural products C1=CC(O)=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O YOOXNSPYGCZLAX-UHFFFAOYSA-N 0.000 description 1
- CFLNHFUPWNRWJA-UHFFFAOYSA-N Obtusin Chemical compound O=C1C2=CC(C)=C(O)C(OC)=C2C(=O)C2=C1C=C(OC)C(OC)=C2O CFLNHFUPWNRWJA-UHFFFAOYSA-N 0.000 description 1
- OBBJQZSMXOJMCN-UHFFFAOYSA-N Obtusin Natural products COc1cc2C=CC(=O)Oc2c3OCC(Oc13)C(=C)C OBBJQZSMXOJMCN-UHFFFAOYSA-N 0.000 description 1
- NTGIIKCGBNGQAR-UHFFFAOYSA-N Rheoemodin Natural products C1=C(O)C=C2C(=O)C3=CC(O)=CC(O)=C3C(=O)C2=C1O NTGIIKCGBNGQAR-UHFFFAOYSA-N 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 230000036772 blood pressure Effects 0.000 description 1
- NZPQWZZXRKZCDU-UHFFFAOYSA-N chrysophanol Natural products Cc1cc(O)c2C(=O)c3c(O)cccc3Oc2c1 NZPQWZZXRKZCDU-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- RHMXXJGYXNZAPX-UHFFFAOYSA-N emodin Chemical compound C1=C(O)C=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O RHMXXJGYXNZAPX-UHFFFAOYSA-N 0.000 description 1
- VASFLQKDXBAWEL-UHFFFAOYSA-N emodin Natural products OC1=C(OC2=C(C=CC(=C2C1=O)O)O)C1=CC=C(C=C1)O VASFLQKDXBAWEL-UHFFFAOYSA-N 0.000 description 1
- 230000001804 emulsifying effect Effects 0.000 description 1
- 230000004438 eyesight Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- PKUBGLYEOAJPEG-UHFFFAOYSA-N physcion Natural products C1=C(C)C=C2C(=O)C3=CC(C)=CC(O)=C3C(=O)C2=C1O PKUBGLYEOAJPEG-UHFFFAOYSA-N 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000008719 thickening Effects 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/48—Fabaceae or Leguminosae (Pea or Legume family); Caesalpiniaceae; Mimosaceae; Papilionaceae
- A61K36/482—Cassia, e.g. golden shower tree
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
- B01D11/0288—Applications, solvents
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- B01D11/028—Flow sheets
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- B01D11/0415—Solvent extraction of solutions which are liquid in combination with membranes
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- C07C46/10—Separation; Purification; Stabilisation; Use of additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
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- C—CHEMISTRY; METALLURGY
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- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B37/00—Preparation of polysaccharides not provided for in groups C08B1/00 - C08B35/00; Derivatives thereof
- C08B37/006—Heteroglycans, i.e. polysaccharides having more than one sugar residue in the main chain in either alternating or less regular sequence; Gellans; Succinoglycans; Arabinogalactans; Tragacanth or gum tragacanth or traganth from Astragalus; Gum Karaya from Sterculia urens; Gum Ghatti from Anogeissus latifolia; Derivatives thereof
- C08B37/0087—Glucomannans or galactomannans; Tara or tara gum, i.e. D-mannose and D-galactose units, e.g. from Cesalpinia spinosa; Tamarind gum, i.e. D-galactose, D-glucose and D-xylose units, e.g. from Tamarindus indica; Gum Arabic, i.e. L-arabinose, L-rhamnose, D-galactose and D-glucuronic acid units, e.g. from Acacia Senegal or Acacia Seyal; Derivatives thereof
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- C07C50/00—Quinones
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Abstract
本发明公开了一种决明子提取物及决明子综合开发利用的工艺技术。所述方法以决明子为原料，采用乙醇提供获得富含总蒽醌的决明子提取物，再将料渣热水提取，提取液采用乙醇‑硫酸铵双水相体系分离精制得到决明子半乳甘露聚糖。本发明同时获得决明子总蒽醌、半乳甘露聚糖两种产品，不仅大大缩短提取时间，而且半乳甘露聚糖提取率高，蛋白含量低设备简单，操作条件温和，不存在除乙醇外的其他有机溶剂残留，应用前景广阔，可实现工业化生产，有利于决明子的开发和综合利用。
Description
技术领域
本发明涉及药食同源原料，具体涉及决明子中有效成分总蒽醌及决明子半乳甘露聚糖的提取制备方法，尤其涉及一种决明子综合开发利用的工艺技术。
技术背景
决明子是国家卫生部公布的药食同源的物质之一,为豆科植物钝叶决明(Cassiaobtusifolia L.)或小决明(Cassia tora L.)的干燥成熟种子,具有降血压、降血脂、明目、抑菌等功效。蒽醌类物质是决明子主要的药用成分，主要包括大黄酚、决明素、大黄素、黄决明素、橙黄决明素等。决明子种同时富含多糖，其主要为半乳甘露聚糖，可作为良好的增稠乳化的食品添加剂。
目前决明子药用成分蒽醌多采用乙醇提取的方法制备，但是存在大量的下角料，造成资源严重浪费。而下角料主要成分为多糖，富含半乳甘露聚糖可作为食品添加剂开发，目前决明子多糖的提取纯化多采用水提醇沉，但仍有大量的杂质，半乳甘露聚糖纯度较低或是决明子分级研磨筛分获得富含多糖的胚乳，然后进行提取异丙醇纯化获得决明子半乳甘露聚糖，工艺复杂且含有异丙醇残留。决明子中药成分蒽醌与半乳甘露聚糖的综合开发并提高产品品质工艺技术是本发明要解决的技术问题。
发明内容
本发明所需要解决的技术问题是：提供一种高品质决明子以及决明子综合利用的工艺技术，同时开发决明子中药成分蒽醌及半乳甘露聚糖，并采用双水相萃取技术获得高品质的决明子半乳甘露聚糖。
本发明提供的决明子提取物中，中药成分蒽醌含量高达4％以上，半乳甘露聚糖含量高达80％以上。
本发明同时提供了所述决明子提取物的制备工艺，即本发明同时提供了一种决明子综合利用的工艺技术，其包括如下步骤：
(1)决明子原料，粉碎得决明子粉末；
(2)决明子浸提：采用乙醇水溶剂进行提取，提取液过滤得决明子提取液，及决明子渣
(3)步骤(2)决明子提取液，真空减压浓缩得浓缩液，浓缩液直接喷雾干燥，得富含蒽醌的决明子提取物；
(4)步骤(2)决明子渣，直接加膜滤水进行提取，离心得上清液；
(5)建立乙醇-硫酸铵双水相体系：离心上清液加入硫酸铵，再加入乙醇形成双水相体系，搅拌均匀，静置分相，半乳甘露聚糖分布于下相；
(6)取下相溶液过滤，将滤液截留分子量为100k的超滤分离，获得决明子半乳甘露聚糖浓缩液。浓缩液真空干燥制得半乳甘露聚糖。
优选的，所述步骤(1)中，决明子粉碎粒度为20-60目。
所述步骤(2)中，乙醇浓度40-85％，加入重量是药材的3-15倍，提取温度20℃-70℃，提取时间0.5-4h，提取次数1-3次；
所述步骤(3)中，旋转蒸发去除过滤液中的乙醇提取溶剂，旋转蒸发的温度为60-80℃，真空度为-0.06-0.095Mpa，浓缩至固形物含量10％-40％；
所述步骤(4)中，料渣加入15-40倍水，优选25倍，提取温度60-100℃，优选90℃；提取时间0.5-3h，优选2h,提取1-2次,优选1次；提取液经高速离心得上清液，离心速率为2000r/min-5000r/min，优选3000r/min；
所述步骤(5)中，所属离心上清液加入硫酸铵，硫酸铵浓度为15-25％，优选23％；再加入乙醇至体积分数为25-35％，优选30％，形成双水相体系；
所述步骤(6)中取下相溶液经200-500目滤布过滤，优选300目，将滤液经截留分子量为50k-200k的超滤膜分离，优选100k；
本发明制备提供一种决明子综合利用的工艺技术，获得的决明子提取物中药成分蒽醌含量4％以上，采用双水相萃取技术获得决明子工艺操作简单可行，适用于工业化生产。
具体实施方式
实施例1：
取决明子原料1kg，制成粗粉，过20目筛，加入70％乙醇6kg,提取温度60℃，搅拌提取2次，每次1h，过滤合并提取液，减压回收乙醇，得固形物含量25％浸膏，直接进行喷雾干燥，得142g决明子提取物，总蒽醌含量5.3％。过滤后的决明子渣加入25倍水，95℃提取2小时，提取1次提取液经3000r/min离心得上清液，离心上清液加入硫酸铵，硫酸铵浓度为23％，再加入乙醇至体积分数为30％，形成双水相体系，搅拌均匀，静置分相，半乳甘露聚糖分布于下相；取下相溶液经300目滤布过滤，将滤液经截留分子量为100k的超滤膜分离，除去小分子及盐杂质，得决明子半乳甘露聚糖浓缩液。浓缩液真空干燥制得半乳甘露聚糖，得率12.3％，半乳甘露聚糖含量84％；
实施例2：
取决明子原料1kg，制成粗粉，过20目筛，加入20％乙醇6kg,提取温度60℃，搅拌提取2次，每次1h，过滤合并提取液，减压回收乙醇，得固形物含量25％浸膏，直接进行喷雾干燥，得189g决明子提取物，总蒽醌含量0.7％。过滤后的决明子渣加入25倍水，95℃提取2小时，提取1次提取液经3000r/min离心得上清液，离心上清液加入硫酸铵，硫酸铵浓度为23％，再加入乙醇至体积分数为30％，形成双水相体系，搅拌均匀，静置分相，半乳甘露聚糖分布于下相；取下相溶液经300目滤布过滤，将滤液经截留分子量为100k的超滤膜分离，除去小分子及盐杂质，得决明子半乳甘露聚糖浓缩液。浓缩液真空干燥制得半乳甘露聚糖，得率9.7％，半乳甘露聚糖含量56％；
实施例3：
取决明子原料1kg，制成粗粉，过20目筛，加入70％乙醇6kg,提取温度60℃，搅拌提取2次，每次1h，过滤合并提取液，减压回收乙醇，得固形物含量25％浸膏，直接进行喷雾干燥，得142g决明子提取物，总蒽醌含量5.3％。过滤后的决明子渣加入25倍水，95℃提取2小时，提取1次提取液经3000r/min离心得上清液，离心上清液加入硫酸铵，硫酸铵浓度为25％，再加入乙醇至体积分数为25％，形成双水相体系，搅拌均匀，静置分相，半乳甘露聚糖分布于下相；取下相溶液经300目滤布过滤，将滤液经截留分子量为100k的超滤膜分离，除去小分子及盐杂质，得决明子半乳甘露聚糖浓缩液。浓缩液真空干燥制得半乳甘露聚糖，得率13.7％，半乳甘露聚糖含量75％；
最后应说明的是：显然，上述实施例仅仅是为清楚地说明本发明所作的举例，而并非对实施方式的限定。对于所属领域的普通技术人员来说，在上述说明的基础上还可以做出其它不同形式的变化或变动。这里无需也无法对所有的实施方式予以穷举。而由此所引伸出的显而易见的变化或变动仍处于本发明的保护范围之中。
Claims (1)
1.一种生产决明子提取物的决明子综合开发利用的工艺技术，其特征在于，该方法包括下列步骤；
(1)决明子原料，粉碎得决明子粉末；
(2)决明子浸提：采用乙醇水溶剂进行提取，提取液过滤得决明子提取液，及决明子渣；
(3)步骤(2)决明子提取液，真空减压浓缩得浓缩液，浓缩液直接喷雾干燥，得富含蒽醌的决明子提取物；
(4)步骤(2)决明子渣，直接加膜滤水进行提取，离心得上清液；
(5)建立乙醇-硫酸铵双水相体系：离心上清液加入硫酸铵，再加入乙醇形成双水相体系，搅拌均匀，静置分相，半乳甘露聚糖分布于下相；
(6)取下相溶液过滤，将滤液截留分子量为100k的超滤分离，获得决明子半乳甘露聚糖浓缩液；浓缩液真空干燥制得半乳甘露聚糖；
其中，所述步骤(1)中，决明子粉碎粒度为20-60目；
所述步骤(2)中，乙醇浓度40-85％，加入重量是药材的3-15倍，提取温度20℃-70℃，提取时间0.5-4h，提取次数1-3次；
所述步骤(3)中，旋转蒸发去除过滤液中的乙醇提取溶剂，旋转蒸发的温度为60-80℃，真空度为-0.06-0.095Mpa，浓缩至固形物含量10％-40％；
所述步骤(4)中，料渣加入25倍水，提取温度90℃；提取时间2h,提取1次；提取液经高速离心得上清液，离心速率为3000r/min；
所述步骤(5)中，所属离心上清液加入硫酸铵，硫酸铵浓度为23％；再加入乙醇至体积分数为30％，形成双水相体系；
所述步骤(6)中，取下相溶液经300目滤布过滤，将滤液经截留分子量为100k的超滤膜分离；
提取物中，中药成分蒽醌含量在4％以上，半乳甘露聚糖含量在80％以上。
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