CN103585187B - A kind of preparation method of wall tapestry extract - Google Patents
A kind of preparation method of wall tapestry extract Download PDFInfo
- Publication number
- CN103585187B CN103585187B CN201310525366.6A CN201310525366A CN103585187B CN 103585187 B CN103585187 B CN 103585187B CN 201310525366 A CN201310525366 A CN 201310525366A CN 103585187 B CN103585187 B CN 103585187B
- Authority
- CN
- China
- Prior art keywords
- extract
- wall coat
- ethanol
- wall
- adsorption resin
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000011347 resin Substances 0.000 claims abstract description 38
- 229920005989 resin Polymers 0.000 claims abstract description 38
- 238000001179 sorption measurement Methods 0.000 claims abstract description 32
- 239000003814 drug Substances 0.000 claims abstract description 12
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 108
- 238000000605 extraction Methods 0.000 claims description 30
- 239000002904 solvent Substances 0.000 claims description 27
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000012141 concentrate Substances 0.000 claims description 21
- 239000000341 volatile oil Substances 0.000 claims description 16
- 238000002791 soaking Methods 0.000 claims description 13
- 229940079593 drug Drugs 0.000 claims description 11
- 229920000858 Cyclodextrin Polymers 0.000 claims description 8
- 239000001116 FEMA 4028 Substances 0.000 claims description 8
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 8
- 235000011175 beta-cyclodextrine Nutrition 0.000 claims description 8
- 229960004853 betadex Drugs 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 8
- 238000001256 steam distillation Methods 0.000 claims description 8
- 238000005057 refrigeration Methods 0.000 claims description 4
- 239000006186 oral dosage form Substances 0.000 abstract description 2
- 239000002994 raw material Substances 0.000 abstract description 2
- 238000007796 conventional method Methods 0.000 abstract 1
- 239000003937 drug carrier Substances 0.000 abstract 1
- 239000000546 pharmaceutical excipient Substances 0.000 abstract 1
- 239000008187 granular material Substances 0.000 description 8
- 239000003480 eluent Substances 0.000 description 6
- 239000000203 mixture Substances 0.000 description 5
- 239000002775 capsule Substances 0.000 description 4
- 229920002472 Starch Polymers 0.000 description 2
- 238000007598 dipping method Methods 0.000 description 2
- -1 dry Substances 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000008107 starch Substances 0.000 description 2
- 235000019698 starch Nutrition 0.000 description 2
- 239000004375 Dextrin Substances 0.000 description 1
- 229920001353 Dextrin Polymers 0.000 description 1
- 229920000168 Microcrystalline cellulose Polymers 0.000 description 1
- 239000002671 adjuvant Substances 0.000 description 1
- 235000019425 dextrin Nutrition 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229930182830 galactose Natural products 0.000 description 1
- 238000003306 harvesting Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 210000004072 lung Anatomy 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 235000019813 microcrystalline cellulose Nutrition 0.000 description 1
- 239000008108 microcrystalline cellulose Substances 0.000 description 1
- 229940016286 microcrystalline cellulose Drugs 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000003826 tablet Substances 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Landscapes
- Medicinal Preparation (AREA)
Abstract
本发明涉及一种壁衣提取物的制备方法，属于医药领域。其制备方法是以壁衣为原料，将壁衣提取后，通过两次大孔吸附树脂纯化得到。可与药学上可接受的载体或其他适宜赋形剂相结合，按照常规方法制成口服给药的剂型。The invention relates to a preparation method of a wall coat extract, which belongs to the field of medicine. The preparation method is to use the wall coat as a raw material, extract the wall coat, and then purify it through two times of macroporous adsorption resin. It can be combined with pharmaceutically acceptable carriers or other suitable excipients, and made into oral dosage forms according to conventional methods.
Description
技术领域 technical field
本发明属于生物医药领域，涉及一种中药材提取物的制备方法，具体是涉及一种壁衣提取物的制备方法。 The invention belongs to the field of biomedicine and relates to a preparation method of an extract of Chinese medicinal materials, in particular to a preparation method of an extract of wall coats.
背景技术 Background technique
壁衣为地衣类黄枝衣科植物壁衣Theloschestes flavicans (Sw.) Norm的干燥叶状体。采集后，除去泥土，晒干。收载于《中华人民共和国卫生部药品标准 藏药（第一册）》，标准编号：WS3-BC-0125-95。性凉，味苦。具有除热，解毒之功效。用于肺热，肝热，脉热，毒热。为我国藏蒙等少数民族地区的常用药物。但有关壁衣的基础研究尚十分有限，使该药材的后续推广和应用受到限制。有关壁衣化学成分及药理作用研究未见报道。 The wall-cover is the dry frond of the lichen-like plant Theloschestes flavicans (Sw.) Norm. After harvesting, the soil is removed and dried in the sun. It is recorded in "Drug Standards of the Ministry of Health of the People's Republic of China Tibetan Medicine (Volume 1)", standard number: WS3-BC-0125-95. Cool in nature, bitter in the mouth. It has the effect of removing heat and detoxifying. For lung heat, liver heat, pulse heat, toxic heat. It is a commonly used drug in ethnic minority areas such as Tibet and Mongolia. However, the basic research on wall coat is still very limited, which limits the subsequent promotion and application of this medicinal material. There is no report on the chemical composition and pharmacological effects of wall coat.
国内专利检索结果，未见壁衣相关专利。 According to domestic patent search results, there is no patent related to wall coverings.
上述文献及专利等，尚未见壁衣提取物制备方法的相关报道。 In the above-mentioned documents and patents, there are no related reports on the preparation method of the wall coat extract.
发明内容 Contents of the invention
本发明的目的在于提供一种壁衣提取物的制备方法。 The purpose of the present invention is to provide a preparation method of wall coat extract.
本发明是通过如下技术方案实现的： The present invention is achieved through the following technical solutions:
本发明所用原料：壁衣为地衣类黄枝衣科植物壁衣Theloschestes flavicans (Sw.) Norm的干燥叶状体。 Raw materials used in the present invention: the wall coat is the dry frond of the lichen class Daffodilaceae plant wall coat Theloschestes flavicans (Sw.) Norm.
本发明一种壁衣提取物的制备方法，其特征在于按以下步骤制备： A preparation method of the wall coat extract of the present invention is characterized in that it is prepared according to the following steps:
（1）壁衣，用浓度90%-100%乙醇作为溶剂，在50℃-70℃温浸提取，提取次数为1-3次，每次提取时间为1-3小时，每次溶剂用量为壁衣重量的10-15倍，滤过，得提取液A和药渣A，提取液A浓缩至无醇清膏，加入蒸馏水，进行水蒸汽蒸馏，收集馏出液，加入馏出液重量4%的β环糊精包合，低温冷藏，过滤，低温干燥，即得壁衣挥发油包合物； (1) For the wall coat, use ethanol with a concentration of 90%-100% as a solvent, and extract it by warm soaking at 50°C-70°C. The number of extractions is 1-3 times, and the extraction time is 1-3 hours each time. The amount of solvent used each time is 10-15 times the weight of the wall coat, filtered to obtain extract A and dregs A, concentrate A to alcohol-free clear paste, add distilled water, carry out steam distillation, collect distillate, add distillate weight 4 % β-cyclodextrin clathrate, refrigerated at low temperature, filtered, and dried at low temperature to obtain the clathrate volatile oil clathrate;
（2）将步骤（1）得到药渣A用浓度20%-70%乙醇为溶剂，在50℃-80℃温浸提取，提取次数为2-5次，每次提取时间为1-6小时，每次溶剂用量为壁衣重量的6-20倍，滤过，提取液回收乙醇，浓缩至相对密度d=1.05-1.18，滤过，得药液B； (2) Use ethanol with a concentration of 20%-70% ethanol as a solvent to obtain the dregs A obtained in step (1), and extract it by warm soaking at 50°C-80°C. The number of extractions is 2-5 times, and the extraction time is 1-6 hours each time. , each time the amount of solvent is 6-20 times of the wall coat weight, filtered, the extract is recovered to ethanol, concentrated to a relative density of d=1.05-1.18, filtered to obtain the medicinal solution B;
（3）将步骤（2）得到的药液B，通过非极性大孔吸附树脂柱，先用水洗脱，水洗脱液直接通过极性大孔树脂柱，再用浓度60%-95%的乙醇溶液洗脱非极性大孔吸附树脂柱，收集不同浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物B；再用浓度60%-95%的乙醇溶液洗脱极性大孔吸附树脂柱，收集不同浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物C； (3) Pass the drug solution B obtained in step (2) through a non-polar macroporous adsorption resin column, and first elute with water, and the water eluent directly passes through the polar macroporous resin column, and then use a concentration of 60%-95% ethanol solution to elute the non-polar macroporous adsorption resin column, collect ethanol eluents of different concentrations, concentrate and dry to obtain wall coat extract B; then elute polar macroporous Adsorption resin column, collecting ethanol eluents with different concentrations, concentrating and drying to obtain wall coat extract C;
（4）上述壁衣挥发油包合物、壁衣提取物A、壁衣提取物B，其中一种或两种或三种按一定比例混匀，即得本发明的壁衣提取物。 (4) The above-mentioned wall coat volatile oil clathrate, wall coat extract A, wall coat extract B, one or two or three of them are mixed in a certain proportion to obtain the wall coat extract of the present invention.
一种壁衣提取物的制备方法，其特征在于按以下步骤制备： A preparation method of wall coat extract, characterized in that it is prepared according to the following steps:
（1）壁衣，用浓度90%-100%乙醇作为溶剂，在50℃-70℃温浸提取，提取次数为1-3次，每次提取时间为1-3小时，每次溶剂用量为壁衣重量的10-15倍，滤过，得提取液A和药渣A，提取液A浓缩至无醇清膏，加入蒸馏水，进行水蒸汽蒸馏，收集馏出液，加入馏出液重量4%的β环糊精包合，低温冷藏，过滤，低温干燥，即得壁衣挥发油包合物； (1) For the wall coat, use ethanol with a concentration of 90%-100% as a solvent, and extract it by warm soaking at 50°C-70°C. The number of extractions is 1-3 times, and the extraction time is 1-3 hours each time. The amount of solvent used each time is 10-15 times the weight of the wall coat, filtered to obtain extract A and dregs A, concentrate A to alcohol-free clear paste, add distilled water, carry out steam distillation, collect distillate, add distillate weight 4 % β-cyclodextrin clathrate, refrigerated at low temperature, filtered, and dried at low temperature to obtain the clathrate volatile oil clathrate;
（2）将步骤（1）得到药渣A用浓度20%-70%乙醇为溶剂，在50℃-80℃温浸提取，提取次数为2-5次，每次提取时间为1-6小时，每次溶剂用量为壁衣重量的6-20倍，滤过，提取液回收乙醇，浓缩至相对密度d=1.05-1.18，滤过，得药液B； (2) Use ethanol with a concentration of 20%-70% ethanol as a solvent to obtain the dregs A obtained in step (1), and extract it by warm soaking at 50°C-80°C. The number of extractions is 2-5 times, and the extraction time is 1-6 hours each time. , each time the amount of solvent is 6-20 times of the wall coat weight, filtered, the extract is recovered to ethanol, concentrated to a relative density of d=1.05-1.18, filtered to obtain the medicinal solution B;
（3）将步骤（2）得到的药液B，通过非极性大孔吸附树脂柱，先用水洗脱，水洗脱液直接通过极性大孔树脂柱，再用浓度60%-95%的乙醇溶液洗脱非极性大孔吸附树脂柱，收集不同浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物B；再用浓度60%-95%的乙醇溶液洗脱极性大孔吸附树脂柱，收集不同浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物C； (3) Pass the drug solution B obtained in step (2) through a non-polar macroporous adsorption resin column, and first elute with water, and the water eluent directly passes through the polar macroporous resin column, and then use a concentration of 60%-95% ethanol solution to elute the non-polar macroporous adsorption resin column, collect ethanol eluents of different concentrations, concentrate and dry to obtain wall coat extract B; then elute polar macroporous Adsorption resin column, collecting ethanol eluents with different concentrations, concentrating and drying to obtain wall coat extract C;
（4）上述壁衣挥发油包合物、壁衣提取物A、壁衣提取物B混匀，即得本发明的壁衣提取物。 (4) The above-mentioned wall coat volatile oil clathrate, wall coat extract A, and wall coat extract B are mixed to obtain the wall coat extract of the present invention.
优选的一种壁衣提取物的制备方法，其特征在于按以下步骤制备： A preferred preparation method of wall coat extract is characterized in that it is prepared according to the following steps:
（1）壁衣，用浓度95%乙醇作为溶剂，在60℃温浸提取，提取次数为2次，每次提取时间为2小时，每次溶剂用量为壁衣重量的12倍，滤过，得提取液A和药渣A，提取液A浓缩至无醇清膏，加入蒸馏水，进行水蒸汽蒸馏，收集馏出液，加入馏出液重量4%的β环糊精包合，低温冷藏，过滤，低温干燥，即得壁衣挥发油包合物； (1) For the wall coat, use 95% ethanol as a solvent, extract by warm soaking at 60°C, the number of extractions is 2 times, each extraction time is 2 hours, and the amount of solvent used each time is 12 times the weight of the wall coat, filtered, Obtain extract A and dregs A, concentrate extract A to alcohol-free clear paste, add distilled water, carry out steam distillation, collect distillate, add β-cyclodextrin clathrate of 4% by weight of distillate, cryogenic refrigeration, Filter and dry at low temperature to obtain the clathrate volatile oil clathrate;
（2）将步骤（1）得到药渣A用浓度50%乙醇为溶剂，在70℃温浸提取，提取次数为3次，每次提取时间为2.5小时，每次溶剂用量为壁衣重量的15倍，滤过，提取液回收乙醇，浓缩至相对密度d=1.12，滤过，得药液B； (2) Use 50% ethanol as the solvent for the dregs A obtained in step (1), and extract by warm soaking at 70°C. The number of extractions is 3 times, and the extraction time is 2.5 hours each time. 15 times, filtered, the extract recovered ethanol, concentrated to a relative density of d=1.12, filtered to obtain the medicinal solution B;
（3）将步骤（2）得到的药液B，通过D101非极性大孔吸附树脂柱，先用水洗脱，水洗脱液直接通过LS-300极性大孔吸附树脂柱，再用浓度70%的乙醇溶液洗脱D101非极性大孔吸附树脂柱，收集70%浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物B；再用浓度95%的乙醇溶液洗脱LS-300极性大孔吸附树脂柱，收集95%浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物C； (3) Pass the drug solution B obtained in step (2) through the D101 non-polar macroporous adsorption resin column, and first elute with water, and the water eluate directly passes through the LS-300 polar macroporous adsorption resin column, and then use the concentration Elute the D101 non-polar macroporous adsorption resin column with 70% ethanol solution, collect the 70% ethanol eluate, concentrate and dry to obtain wall coat extract B; then elute LS-300 with 95% ethanol solution Polar macroporous adsorption resin column, collect 95% ethanol eluate, concentrate and dry to obtain wall coat extract C;
（4）上述壁衣挥发油包合物、壁衣提取物A、壁衣提取物B，混匀，即得本发明的壁衣提取物。 (4) The above-mentioned wall coat volatile oil clathrate, wall coat extract A, and wall coat extract B are mixed evenly to obtain the wall coat extract of the present invention.
本发明的一种壁衣提取物的制备方法，其特征在于：所采用的非极性大孔吸附树脂为AB-8大孔吸附树脂、D101大孔吸附树脂；所采用的极性大孔吸附树脂为LS-300大孔吸附树脂、HPD600大孔吸附树脂。 A kind of preparation method of wall coat extract of the present invention is characterized in that: the non-polar macroporous adsorption resin that adopts is AB-8 macroporous adsorption resin, D101 macroporous adsorption resin; The resins are LS-300 macroporous adsorption resin and HPD600 macroporous adsorption resin.
本发明的壁衣提取物，通过加入药剂学允许的各种辅料，制成药剂学上的片剂、颗粒剂、胶囊剂等口服剂型。 The wall coat extract of the present invention is prepared into pharmaceutical oral dosage forms such as tablets, granules, and capsules by adding various pharmaceutically acceptable adjuvants.
具体实施方式 Detailed ways
下面通过具体实验例和实施例对本发明的一种壁衣提取物的制备方法做进一步说明，但不限于本发明。 The preparation method of a wall coat extract of the present invention will be further described through specific experimental examples and examples below, but it is not limited to the present invention.
下面通过具体实施例作进一步详述。 Further details are given below through specific examples.
实施例1：壁衣提取物的制备 Embodiment 1: the preparation of wall coat extract
（1）壁衣15kg，用浓度95%乙醇作为溶剂，在60℃温浸提取，提取次数为2次，每次提取时间为2小时，每次溶剂用量为壁衣重量的12倍，滤过，得提取液A和药渣A，提取液A浓缩至无醇清膏，加入蒸馏水，进行水蒸汽蒸馏，收集馏出液，加入馏出液重量4%的β环糊精包合，低温冷藏，过滤，低温干燥，即得壁衣挥发油包合物； (1) 15 kg of wall coat, use 95% ethanol as solvent, warm soak and extract at 60°C, the number of extractions is 2 times, each extraction time is 2 hours, the amount of solvent for each time is 12 times the weight of the wall coat, filter , to obtain extract A and dregs A, concentrate extract A to alcohol-free clear paste, add distilled water, carry out steam distillation, collect distillate, add β-cyclodextrin clathrate of 4% by weight of distillate, and refrigerate , filtered, and dried at low temperature to obtain the clathrate of the wall coat volatile oil;
（2）将步骤（1）得到药渣A用浓度50%乙醇为溶剂，在70℃温浸提取，提取次数为3次，每次提取时间为2.5小时，每次溶剂用量为壁衣重量的15倍，滤过，提取液回收乙醇，浓缩至相对密度d=1.12，滤过，得药液B； (2) Use 50% ethanol as the solvent for the dregs A obtained in step (1), and extract by warm soaking at 70°C. The number of extractions is 3 times, and the extraction time is 2.5 hours each time. 15 times, filtered, the extract recovered ethanol, concentrated to a relative density of d=1.12, filtered to obtain the medicinal solution B;
（3）将步骤（2）得到的药液B，通过D101非极性大孔吸附树脂柱，先用水洗脱，水洗脱液直接通过LS-300极性大孔吸附树脂柱，再用浓度70%的乙醇溶液洗脱D101非极性大孔吸附树脂柱，收集70%浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物B；再用浓度95%的乙醇溶液洗脱LS-300极性大孔吸附树脂柱，收集95%浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物C； (3) Pass the drug solution B obtained in step (2) through the D101 non-polar macroporous adsorption resin column, and first elute with water, and the water eluate directly passes through the LS-300 polar macroporous adsorption resin column, and then use the concentration Elute the D101 non-polar macroporous adsorption resin column with 70% ethanol solution, collect the 70% ethanol eluate, concentrate and dry to obtain wall coat extract B; then elute LS-300 with 95% ethanol solution Polar macroporous adsorption resin column, collect 95% ethanol eluate, concentrate and dry to obtain wall coat extract C;
（4）上述壁衣挥发油包合物、壁衣提取物A、壁衣提取物B，混匀，即得本发明的壁衣提取物。 (4) The above-mentioned wall coat volatile oil clathrate, wall coat extract A, and wall coat extract B are mixed evenly to obtain the wall coat extract of the present invention.
实施例2：壁衣提取物的制备 Embodiment 2: the preparation of wall coat extract
（1）壁衣20kg，用浓度90%乙醇作为溶剂，在70℃温浸提取，提取次数为1次，每次提取时间为3小时，每次溶剂用量为壁衣重量的15倍，滤过，得提取液A和药渣A，提取液A浓缩至无醇清膏，加入蒸馏水，进行水蒸汽蒸馏，收集馏出液，加入馏出液重量4%的β环糊精包合，低温冷藏，过滤，低温干燥，即得壁衣挥发油包合物； (1) 20kg of wall coat, using 90% ethanol as solvent, warm soaking and extracting at 70°C, the number of extractions is 1 time, each extraction time is 3 hours, and the amount of solvent used each time is 15 times the weight of the wall coat, and filtered , to obtain extract A and dregs A, concentrate extract A to alcohol-free clear paste, add distilled water, carry out steam distillation, collect distillate, add β-cyclodextrin clathrate of 4% by weight of distillate, and refrigerate , filtered, and dried at low temperature to obtain the clathrate of the wall coat volatile oil;
（2）将步骤（1）得到药渣A用浓度70%乙醇为溶剂，在50℃温浸提取，提取次数为5次，每次提取时间为1小时，每次溶剂用量为壁衣重量的6倍，滤过，提取液回收乙醇，浓缩至相对密度d=1.05，滤过，得药液B； (2) Use 70% ethanol as a solvent to extract the medicinal dregs A obtained in step (1), warm soaking and extracting at 50°C, the number of extractions is 5 times, each extraction time is 1 hour, and the amount of solvent used each time is 100% of the weight of the wall coat 6 times, filtered, the extract recovered ethanol, concentrated to a relative density of d=1.05, filtered to obtain the medicinal solution B;
（3）将步骤（2）得到的药液B，通过AB-8非极性大孔吸附树脂柱，先用水洗脱，水洗脱液直接通过HPD600极性大孔树脂柱，再用浓度60%的乙醇溶液洗脱AB-8非极性大孔吸附树脂柱，收集60%浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物B；再用浓度95%的乙醇溶液洗脱HPD600极性大孔吸附树脂柱，收集95%浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物C； (3) Pass the drug solution B obtained in step (2) through the AB-8 non-polar macroporous adsorption resin column, and first elute with water, and the water eluate directly passes through the HPD600 polar macroporous resin column, and then use a concentration of 60 % ethanol solution to elute AB-8 non-polar macroporous adsorption resin column, collect 60% ethanol eluate, concentrate and dry to obtain wall coat extract B; then elute HPD600 electrode with 95% ethanol solution Macroporous adsorption resin column, collect 95% ethanol eluate, concentrate and dry to obtain wall coat extract C;
（4）上述壁衣挥发油包合物、壁衣提取物A、壁衣提取物B混匀，即得本发明的壁衣提取物。 (4) The above-mentioned wall coat volatile oil clathrate, wall coat extract A, and wall coat extract B are mixed to obtain the wall coat extract of the present invention.
实施例3：壁衣提取物的制备 Embodiment 3: the preparation of wall coat extract
（1）壁衣30kg，用100%乙醇作为溶剂，在50℃温浸提取，提取次数为3次，每次提取时间为1小时，每次溶剂用量为壁衣重量的10倍，滤过，得提取液A和药渣A，提取液A浓缩至无醇清膏，加入蒸馏水，进行水蒸汽蒸馏，收集馏出液，加入馏出液重量4%的β环糊精包合，低温冷藏，过滤，低温干燥，即得壁衣挥发油包合物； (1) 30kg of wall coat, use 100% ethanol as solvent, extract by warm dipping at 50°C, the number of extractions is 3 times, each extraction time is 1 hour, the amount of solvent for each time is 10 times the weight of the wall coat, filter, Obtain extract A and dregs A, concentrate extract A to alcohol-free clear paste, add distilled water, carry out steam distillation, collect distillate, add β-cyclodextrin clathrate of 4% by weight of distillate, cryogenic refrigeration, Filter and dry at low temperature to obtain the clathrate volatile oil clathrate;
（2）将步骤（1）得到药渣A用浓度20%乙醇为溶剂，在80℃温浸提取，提取次数为2次，每次提取时间为6小时，每次溶剂用量为壁衣重量的20倍，滤过，提取液回收乙醇，浓缩至相对密度d=1.18，滤过，得药液B； (2) Use 20% ethanol as a solvent to extract the medicinal dregs A obtained in step (1), and extract them by warm soaking at 80°C. 20 times, filter, recover ethanol from the extract, concentrate to a relative density of d=1.18, filter to obtain medicinal solution B;
（3）将步骤（2）得到的药液B，通过D101非极性大孔吸附树脂柱，先用水洗脱，水洗脱液直接通过HPD600极性大孔树脂柱，再用浓度95%的乙醇溶液洗脱D101非极性大孔吸附树脂柱，收集95%浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物B；再用浓度60%的乙醇溶液洗脱HPD600极性大孔吸附树脂柱，收集60%浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物C； (3) Pass the drug solution B obtained in step (2) through the D101 non-polar macroporous adsorption resin column, and first elute with water, and the water eluate directly passes through the HPD600 polar macroporous resin column, and then use 95% concentration of Elute D101 non-polar macroporous adsorption resin column with ethanol solution, collect 95% ethanol eluate, concentrate and dry to obtain wall coat extract B; then elute HPD600 polar macroporous adsorption resin with 60% ethanol solution Resin column, collect 60% ethanol eluate, concentrate and dry to obtain wall coat extract C;
（4）上述壁衣挥发油包合物、壁衣提取物A、壁衣提取物B混匀，即得本发明的壁衣提取物。 (4) The above-mentioned wall coat volatile oil clathrate, wall coat extract A, and wall coat extract B are mixed to obtain the wall coat extract of the present invention.
实施例4：壁衣提取物的制备 Embodiment 4: the preparation of wall coat extract
（1）壁衣18kg，用95%乙醇作为溶剂，在65℃温浸提取，提取次数为2次，每次提取时间为3小时，每次溶剂用量为壁衣重量的11倍，滤过，得提取液A和药渣A，提取液A浓缩至无醇清膏，加入蒸馏水，进行水蒸汽蒸馏，收集馏出液，加入馏出液重量4%的β环糊精包合，低温冷藏，过滤，低温干燥，即得壁衣挥发油包合物； (1) 18 kg of wall coat, use 95% ethanol as solvent, extract by warm dipping at 65°C, the number of extractions is 2 times, each extraction time is 3 hours, the amount of solvent for each time is 11 times the weight of the wall coat, filter, Obtain extract A and dregs A, concentrate extract A to alcohol-free clear paste, add distilled water, carry out steam distillation, collect distillate, add β-cyclodextrin clathrate of 4% by weight of distillate, cryogenic refrigeration, Filter and dry at low temperature to obtain the clathrate volatile oil clathrate;
（2）将步骤（1）得到药渣A用浓度40%乙醇为溶剂，在70℃温浸提取，提取次数为4次，每次提取时间为3小时，每次溶剂用量为壁衣重量的15倍，滤过，提取液回收乙醇，浓缩至相对密度d=1.14，滤过，得药液B； (2) Use 40% ethanol as a solvent to extract the medicinal dregs A obtained in step (1), and extract by warm soaking at 70°C. The number of extractions is 4 times, and the extraction time is 3 hours each time. 15 times, filtered, the extract recovered ethanol, concentrated to relative density d=1.14, filtered to obtain liquid B;
（3）将步骤（2）得到的药液B，通过D101非极性大孔吸附树脂柱，用水洗脱，再用浓度85%的乙醇溶液D101洗脱非极性大孔吸附树脂柱，收集85%浓度乙醇洗脱液，浓缩干燥，即得壁衣提取物A； (3) Pass the drug solution B obtained in step (2) through the D101 non-polar macroporous adsorption resin column, elute with water, and then use 85% ethanol solution D101 to elute the non-polar macroporous adsorption resin column, collect 85% ethanol eluate, concentrated and dried to obtain the wall coat extract A;
（4）上述壁衣挥发油包合物、壁衣提取物A混匀，即得本发明的壁衣提取物。 (4) The above-mentioned wall coat volatile oil clathrate and wall coat extract A are mixed to obtain the wall coat extract of the present invention.
实施例5: 壁衣提取物片剂的制备 Embodiment 5: the preparation of wall coat extract tablet
取实施例1壁衣提取物265g，加入淀粉62g，混匀，制粒，干燥，过筛，加微晶纤维素15g，硬脂酸镁0.5g，混匀，压制成1000片, 即得壁衣提取物片剂。 Take 265g of the wall coat extract of Example 1, add 62g of starch, mix well, granulate, dry, sieve, add 15g of microcrystalline cellulose, 0.5g of magnesium stearate, mix well, press into 1000 pieces, and get the wall coat Coat Extract Tablets.
实施例6：壁衣提取物颗粒剂的制备 Embodiment 6: the preparation of wall coat extract granule
取实施例2壁衣提取物250g，加入糊精120g，混匀，制粒，干燥，整粒，即成得壁衣提取物颗粒剂。 Take 250 g of the wall coat extract of Example 2, add 120 g of dextrin, mix evenly, granulate, dry, and granulate to obtain the wall coat extract granule.
实施例7：壁衣提取物胶囊的制备 Embodiment 7: the preparation of wall coat extract capsule
取实施例3壁衣提取物275g，加入淀粉35g，半乳糖40g，混匀，制粒，干燥，整粒，装胶囊1000粒，即得壁衣提取物胶囊。 Take 275 g of the wall coat extract of Example 3, add 35 g of starch and 40 g of galactose, mix evenly, granulate, dry, granulate, and pack 1000 capsules to obtain the wall coat extract capsules.
Claims (1)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525366.6A CN103585187B (en) | 2013-10-31 | 2013-10-31 | A kind of preparation method of wall tapestry extract |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310525366.6A CN103585187B (en) | 2013-10-31 | 2013-10-31 | A kind of preparation method of wall tapestry extract |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103585187A CN103585187A (en) | 2014-02-19 |
| CN103585187B true CN103585187B (en) | 2015-08-26 |
Family
ID=50075641
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310525366.6A Expired - Fee Related CN103585187B (en) | 2013-10-31 | 2013-10-31 | A kind of preparation method of wall tapestry extract |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103585187B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106617042A (en) * | 2016-09-13 | 2017-05-10 | 防城港市天红农业科技有限责任公司 | Preparation method of syzygium samarangense extract |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1698769A (en) * | 2005-05-17 | 2005-11-23 | 重庆医药工业研究院有限责任公司 | Bupleurum root soft capsule and its preparation method |
| CN101357146A (en) * | 2008-06-17 | 2009-02-04 | 江西天佑药业有限公司 | Preparation method of chimonanthus nitens valid target, production method and use of formulation thereof |
| CN102671017A (en) * | 2012-04-27 | 2012-09-19 | 湖北长友现代农业股份有限公司 | Method for simultaneously preparing indocalamus leaf volatile oil, total flavone and total polysaccharide |
| CN102670727A (en) * | 2011-03-18 | 2012-09-19 | 山西振东开元制药有限公司 | Forsythia suspense soft capsule, preparation method and application thereof |
-
2013
- 2013-10-31 CN CN201310525366.6A patent/CN103585187B/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1698769A (en) * | 2005-05-17 | 2005-11-23 | 重庆医药工业研究院有限责任公司 | Bupleurum root soft capsule and its preparation method |
| CN101357146A (en) * | 2008-06-17 | 2009-02-04 | 江西天佑药业有限公司 | Preparation method of chimonanthus nitens valid target, production method and use of formulation thereof |
| CN102670727A (en) * | 2011-03-18 | 2012-09-19 | 山西振东开元制药有限公司 | Forsythia suspense soft capsule, preparation method and application thereof |
| CN102671017A (en) * | 2012-04-27 | 2012-09-19 | 湖北长友现代农业股份有限公司 | Method for simultaneously preparing indocalamus leaf volatile oil, total flavone and total polysaccharide |
Non-Patent Citations (2)
| Title |
|---|
| "吴茱萸药材水蒸气蒸馏-醇提过大孔树脂柱联用工艺研究";张军等;《食品与药品》;20091231;第11卷(第03期);12-14 * |
| 中华人民共和国卫生部药典委员会编."壁衣".《中华人民共和国卫生部药品标准 藏药(第一册)》.1995, * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106617042A (en) * | 2016-09-13 | 2017-05-10 | 防城港市天红农业科技有限责任公司 | Preparation method of syzygium samarangense extract |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103585187A (en) | 2014-02-19 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102976909B (en) | Method for extracting and purifying 6-gingerol from ginger | |
| CN103585311B (en) | A kind of preparation method of Spiraea alpina extract | |
| CN101797447A (en) | Method for separating and purifying effective ingredients in natural product | |
| CN101037467B (en) | Method for separating and purifying ursolic acid from loquat leaves | |
| CN104435226A (en) | Paederia scandens extract and application thereof | |
| CN102219814A (en) | Method for extracting aucubin from eucommia ulmoides oliver seed draff | |
| CN103848740A (en) | Method for preparing rosmarinic acid from vegetable oil meal | |
| CN101234147B (en) | Method of preparing total flavones of tropaeolum for injections | |
| CN102805767B (en) | Heat stranguria removal granule raw material polygonum capitatum extract with anti-gonococcus effect | |
| CN103664987B (en) | Artemisinin and preparation method thereof | |
| CN103585187B (en) | A kind of preparation method of wall tapestry extract | |
| CN105175426B (en) | A kind of method of the extraction purification Bergenin from treebine stem | |
| CN107722080A (en) | A kind of method that ursin is extracted in the leaf from purple bergenia herb | |
| CN103484254A (en) | Method for extraction of ligusticum chuanxiong hort. volatile oil by utilizing supercritical carbon dioxide | |
| CN104546952B (en) | A kind of selaginella doederlleini active component and its production and use | |
| CN109721583A (en) | A kind of preparation method of aristolochic acid A and Aristolochic acid B C standard items | |
| CN101531665A (en) | Purification method of psoralen and isopsoralen | |
| CN104107225B (en) | Chinese crude drug Radix Polygalae anticoagulation effective site and extracting method thereof and application | |
| CN102697827B (en) | Coumarin from Cichorium plants used for preparing drug with liver-protecting effect, and extraction and purification method of coumarin from Cichorium plants | |
| CN103585210B (en) | The preparation method of Dorema ammoniacum resin total sesquiterpene coumarin extract | |
| CN102805759B (en) | Total flavone of Hypericum ascyron L and extraction method and application thereof | |
| CN206143103U (en) | Very heavy genistein and genistin extraction system of pulling out of da ye | |
| CN101278980A (en) | A kind of quaternary ammonium total alkali and preparation method thereof | |
| CN103933122B (en) | A kind of adsorbing separation preparation technology of magnolia bark total-phenol extract | |
| CN103772338A (en) | Vacuum pulse type method of preparing dihydromyricetin |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| ASS | Succession or assignment of patent right |
Owner name: JILIN UNIVERSITY Free format text: FORMER OWNER: JINAN XINGYI MEDICAL TECHNOLOGY CO., LTD. Effective date: 20150728 |
|
| C41 | Transfer of patent application or patent right or utility model | ||
| C53 | Correction of patent for invention or patent application | ||
| CB03 | Change of inventor or designer information |
Inventor after: Cheng Guanghui Inventor after: Mao Jincheng Inventor after: Li Fei Inventor before: Kong Qianqian |
|
| COR | Change of bibliographic data |
Free format text: CORRECT: INVENTOR; FROM: KONG QIANQIAN TO: CHENG GUANGHUI MAO JINCHENG LI FEI |
|
| TA01 | Transfer of patent application right |
Effective date of registration: 20150728 Address after: 130012 Changchun Qianjin Street, Jilin, No. 2699 Applicant after: Jilin University Address before: 250101 No. 51 Industrial South Road, Ji'nan hi tech Zone, Shandong, Ji'nan Applicant before: Jinan Xingyi Medical Technology Co.,Ltd. |
|
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20150826 Termination date: 20161031 |
|
| CF01 | Termination of patent right due to non-payment of annual fee |