CN101857644A - Alcohol-Alkali Extraction and Production Technology of Asparagine Polysaccharide - Google Patents
Alcohol-Alkali Extraction and Production Technology of Asparagine Polysaccharide Download PDFInfo
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- CN101857644A CN101857644A CN 201010180715 CN201010180715A CN101857644A CN 101857644 A CN101857644 A CN 101857644A CN 201010180715 CN201010180715 CN 201010180715 CN 201010180715 A CN201010180715 A CN 201010180715A CN 101857644 A CN101857644 A CN 101857644A
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- 229920001282 polysaccharide Polymers 0.000 title claims abstract description 31
- 239000005017 polysaccharide Substances 0.000 title claims abstract description 31
- 238000000605 extraction Methods 0.000 title claims abstract description 30
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 12
- 239000003513 alkali Substances 0.000 title claims abstract description 11
- -1 Asparagine Polysaccharide Chemical class 0.000 title description 13
- DCXYFEDJOCDNAF-UHFFFAOYSA-N Asparagine Natural products OC(=O)C(N)CC(N)=O DCXYFEDJOCDNAF-UHFFFAOYSA-N 0.000 title description 9
- 229960001230 asparagine Drugs 0.000 title description 9
- 235000009582 asparagine Nutrition 0.000 title description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 48
- 150000004676 glycans Chemical class 0.000 claims abstract description 18
- 239000006228 supernatant Substances 0.000 claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- 238000001556 precipitation Methods 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000002904 solvent Substances 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims abstract 2
- 238000000034 method Methods 0.000 claims description 12
- 239000012141 concentrate Substances 0.000 claims description 5
- 239000003814 drug Substances 0.000 claims description 4
- 229940079593 drug Drugs 0.000 claims description 3
- 239000007788 liquid Substances 0.000 claims description 2
- 229960004756 ethanol Drugs 0.000 claims 3
- 229960000935 dehydrated alcohol Drugs 0.000 claims 1
- 241000234427 Asparagus Species 0.000 abstract description 18
- 235000005340 Asparagus officinalis Nutrition 0.000 abstract description 18
- 239000000284 extract Substances 0.000 abstract description 18
- 239000002244 precipitate Substances 0.000 abstract description 7
- 238000005119 centrifugation Methods 0.000 abstract description 2
- 238000003809 water extraction Methods 0.000 description 8
- 108010011485 Aspartame Proteins 0.000 description 4
- 229960003438 aspartame Drugs 0.000 description 4
- 235000010357 aspartame Nutrition 0.000 description 4
- 239000000605 aspartame Substances 0.000 description 4
- 102000011759 adducin Human genes 0.000 description 3
- 108010076723 adducin Proteins 0.000 description 3
- 239000012153 distilled water Substances 0.000 description 3
- 229960005486 vaccine Drugs 0.000 description 3
- 241000287828 Gallus gallus Species 0.000 description 2
- 244000248539 Asparagus cochinchinensis Species 0.000 description 1
- 235000009292 Asparagus cochinchinensis Nutrition 0.000 description 1
- 208000035240 Disease Resistance Diseases 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 239000003623 enhancer Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- OQUKIQWCVTZJAF-UHFFFAOYSA-N phenol;sulfuric acid Chemical compound OS(O)(=O)=O.OC1=CC=CC=C1 OQUKIQWCVTZJAF-UHFFFAOYSA-N 0.000 description 1
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- Polysaccharides And Polysaccharide Derivatives (AREA)
Abstract
本发明公开了一种天门冬多糖的醇碱提取法和生产工艺。提取法如下:取天门冬饮片,按质量体积比1∶15~1∶6加入乙醇浓度为5~50%的提取溶剂,调节pH至5~13,浸泡0.5~2.5小时后于水浴60~100℃提取0.5~2.5小时,过滤,残渣同上处理至少一次,合并各次滤液得提取液。采用该提取法的生产工艺还包括如下:浓缩提取液,加入95%乙醇进行醇沉,弃掉上清;加入同浓缩液量的水加热溶解沉淀,离心收集上清;再加入体积5倍于浓缩液的95%乙醇进行醇沉,离心弃掉上清;加入适量95%乙醇搅匀,离心再弃上清;加适量无水乙醇搅匀,离心后收集沉淀,冷冻干燥即得。本发明显著地提高了天门冬多糖提取率和总糖含量。The invention discloses an alcohol-alkali extraction method and a production process of asparagus polysaccharide. The extraction method is as follows: take asparagus decoction pieces, add an extraction solvent with an ethanol concentration of 5 to 50% according to the mass volume ratio of 1:15 to 1:6, adjust the pH to 5 to 13, soak for 0.5 to 2.5 hours, and place it in a water bath of 60 to 100 Extract at ℃ for 0.5-2.5 hours, filter, treat the residue at least once as above, and combine the filtrates to obtain the extract. The production process adopting this extraction method also includes the following steps: concentrating the extract, adding 95% ethanol for alcohol precipitation, discarding the supernatant; adding the same amount of water as the concentrated solution, heating and dissolving the precipitate, and centrifuging to collect the supernatant; Precipitate with 95% ethanol in the concentrated solution, centrifuge and discard the supernatant; add an appropriate amount of 95% ethanol to stir, centrifuge and then discard the supernatant; add an appropriate amount of absolute ethanol to stir, collect the precipitate after centrifugation, and freeze-dry. The invention obviously improves the extraction rate and total sugar content of the asparagus polysaccharide.
Description
技术领域technical field
本发明涉及一种天门冬多糖的醇碱提取法和生产工艺。The invention relates to an alcohol-alkali extraction method and a production process of aspartame polysaccharide.
背景技术Background technique
天门冬多糖(Asparagus Cochinchinensis polysaccharide)作为鸡的疫苗免疫增强剂,可显著提高疫苗的保护率和抗病力,应用前景广阔。然而,目前提取天门冬多糖的经典水提法和碱水提取法存在提取率低和总糖含量低的问题,以致于天门冬多糖的生产效率低、供应不足,难以满足市场需求。Asparagus Cochinchinensis polysaccharide, as a chicken vaccine immune enhancer, can significantly improve the protection rate and disease resistance of the vaccine, and has a broad application prospect. However, the current classical water extraction and alkaline water extraction methods for extracting asparagus polysaccharides have the problems of low extraction rate and low total sugar content, so that the production efficiency of asparagus polysaccharides is low and the supply is insufficient, making it difficult to meet market demand.
发明内容Contents of the invention
本发明要解决的技术问题是提供一种提取率高和总糖含量高的天门冬多糖的醇碱提取法和生产工艺。The technical problem to be solved by the present invention is to provide an alcohol-alkali extraction method and production process of aspartame polysaccharide with high extraction rate and high total sugar content.
为解决上述技术问题本发明的天门冬多糖的醇碱提取法采用如下技术方案:取天门冬饮片,按质量体积比1∶15~1∶6加入乙醇浓度为5~50%的提取溶剂,调节pH至5~13,浸泡0.5~2.5小时后于水浴60~100℃提取0.5~2.5小时,过滤,残渣同上处理至少一次,合并各次滤液得提取液。In order to solve the above-mentioned technical problems, the alcohol-alkali extraction method of asparagus polysaccharide of the present invention adopts following technical scheme: get asparagus decoction pieces, add the extraction solvent that ethanol concentration is 5~50% by mass volume ratio 1: 15~1: 6, adjust pH to 5-13, soak for 0.5-2.5 hours, then extract in a water bath at 60-100°C for 0.5-2.5 hours, filter, treat the residue at least once as above, and combine the filtrates to obtain the extract.
采用上述醇碱提取法的天门冬多糖的生产工艺,还包括如下步骤:浓缩提取液至含生药0.5g/ml得浓缩液,加入体积5倍于浓缩液的95%乙醇进行醇沉,弃掉上清;加入同浓缩液量的水加热溶解沉淀,离心收集上清;再加入体积5倍于浓缩液的95%乙醇进行醇沉,离心弃掉上清;加入适量95%乙醇搅匀,离心再弃上清;加适量无水乙醇搅匀,离心后收集沉淀,冷冻干燥即得天门冬多糖。The production technology of asparagus polysaccharide adopting the above-mentioned alcohol-alkali extraction method also includes the following steps: concentrating the extract to obtain a concentrated solution containing 0.5g/ml crude drug, adding 95% ethanol with a volume 5 times that of the concentrated solution for alcohol precipitation, discarding Supernatant; add the same amount of water as the concentrate, heat to dissolve the precipitate, centrifuge to collect the supernatant; then add 95% ethanol with a volume 5 times that of the concentrate for alcohol precipitation, centrifuge and discard the supernatant; add an appropriate amount of 95% ethanol to stir well, and centrifuge Then discard the supernatant; add an appropriate amount of absolute ethanol to stir evenly, collect the precipitate after centrifugation, and freeze-dry to obtain asparagine polysaccharide.
本发明的天门冬多糖的醇碱提取法和生产工艺的提取率和总糖含量均高于目前的经典水提法和碱水提取法,应用于生产天门冬多糖可提高效率、满足市场需求。The extraction rate and total sugar content of the alcohol-alkali extraction method and the production process of the asparagine polysaccharide of the present invention are higher than the current classic water extraction method and alkaline water extraction method, and the application to the production of the asparagine polysaccharide can improve efficiency and meet market demand.
具体实施方式Detailed ways
以下为本发明天门冬多糖的醇碱提取法的实施例:Below is the embodiment of the alcohol-alkali extraction method of aspartame polysaccharide of the present invention:
实施例1Example 1
取烘干至恒重的中药天门冬饮片100g,加入乙醇浓度为10%的提取溶剂1500ml,调节pH至9,浸泡1.5小时后于水浴80℃提取2.5小时,四层纱布过滤,残渣同上处理一次,合并两次滤液得提取液。Take 100g of Asparagus decoction pieces dried to constant weight, add 1500ml of extraction solvent with ethanol concentration of 10%, adjust pH to 9, soak for 1.5 hours, extract in water bath at 80°C for 2.5 hours, filter with four layers of gauze, and treat the residue once as above , Combine the two filtrates to obtain the extract.
实施例2Example 2
取烘干至恒重的中药天门冬饮片100g,加入乙醇浓度为5%的提取溶剂600ml,调节pH至13,浸泡2.5小时后于水浴60℃提取1.5小时,四层纱布过滤,残渣同上处理一次,合并两次滤液得提取液。Take 100g of Asparagus decoction pieces dried to constant weight, add 600ml of extraction solvent with ethanol concentration of 5%, adjust the pH to 13, soak for 2.5 hours, extract in water bath at 60°C for 1.5 hours, filter with four layers of gauze, and treat the residue once as above , Combine the two filtrates to obtain the extract.
实施例3Example 3
取烘干至恒重的中药天门冬饮片100g,加入乙醇浓度为30%的提取溶剂1000ml,调节pH至5,浸泡0.5小时后于水浴100℃提取0.5小时,四层纱布过滤,残渣同上处理一次,合并两次滤液得提取液。Take 100g of Asparagus decoction pieces dried to constant weight, add 1000ml of extraction solvent with ethanol concentration of 30%, adjust pH to 5, soak for 0.5 hours, extract in water bath at 100°C for 0.5 hours, filter with four layers of gauze, and treat the residue once as above , Combine the two filtrates to obtain the extract.
实施例4Example 4
取烘干至恒重的中药天门冬饮片100g,加入乙醇浓度为50%的提取溶剂800ml,调节pH至7,浸泡2.0小时后于水浴90℃提取1.0小时,四层纱布过滤,残渣同上处理一次,合并两次滤液得提取液。Take 100g of Asparagus decoction pieces dried to constant weight, add 800ml of extraction solvent with ethanol concentration of 50%, adjust pH to 7, soak for 2.0 hours, extract in water bath at 90°C for 1.0 hour, filter with four layers of gauze, and treat the residue once as above , Combine the two filtrates to obtain the extract.
以下为天门冬多糖的经典水提法和碱水提取法的对照例:The following is a comparison example of the classic water extraction method and alkaline water extraction method of aspartame polysaccharide:
对照1天门冬多糖的经典水提法The classic water extraction method of control 1 asparagine polysaccharide
取烘干至恒重的中药天门冬饮片100g,加入蒸馏水1500ml后煎煮提取2.5小时,四层纱布过滤,残渣同上处理一次,合并两次滤液得提取液。Take 100 g of Radix Asparagus decoction pieces dried to constant weight, add 1500 ml of distilled water, decoct and extract for 2.5 hours, filter through four layers of gauze, treat the residue once as above, and combine the two filtrates to obtain the extract.
对照2天门冬多糖的碱水提取法Alkaline Water Extraction Method of Control 2 Asparagine Polysaccharide
取烘干至恒重的中药天门冬饮片100g,加入蒸馏水1500ml,调节pH至9,浸泡1.5小时后于水浴80℃提取2.5小时,四层纱布过滤,残渣同上处理一次,合并两次滤液得提取液。Take 100g of Asparagus decoction pieces dried to constant weight, add 1500ml of distilled water, adjust the pH to 9, soak for 1.5 hours, then extract in a water bath at 80°C for 2.5 hours, filter through four layers of gauze, treat the residue once as above, and combine the two filtrates to obtain the extraction liquid.
实施例5天门冬多糖的生产工艺The production technology of embodiment 5 asparagine polysaccharides
分别浓缩上述实施例1至4和对照1及2的提取液至含生药0.5g/ml得浓缩液200ml,加入体积5倍于浓缩液的95%乙醇进行醇沉,缓慢加入,边加边搅拌,室温静置过夜,随后弃掉上清;加入200mL蒸馏水加热溶解沉淀,3000r/min离心10min,收集上清;再加入体积5倍于浓缩液的95%乙醇进行醇沉,室温放置过夜,3000r/min离心10min,弃上清;加入适量95%乙醇搅匀,离心同前,再弃上清;加适量无水乙醇搅匀,再离心,最后收集沉淀,冷冻干燥后即得天门冬多糖。Concentrate the extracts of the above-mentioned Examples 1 to 4 and Controls 1 and 2 respectively to contain 0.5 g/ml of crude drug to obtain 200 ml of concentrated solution, add 95% ethanol with a volume 5 times that of the concentrated solution for alcohol precipitation, add slowly, and stir while adding , stand overnight at room temperature, then discard the supernatant; add 200mL of distilled water to heat to dissolve the precipitate, centrifuge at 3000r/min for 10min, and collect the supernatant; then add 95% ethanol with a volume 5 times that of the concentrated solution for alcohol precipitation, place at room temperature overnight, 3000r Centrifuge for 10 min at 1/min, discard the supernatant; add an appropriate amount of 95% ethanol and stir evenly, centrifuge as before, then discard the supernatant; add appropriate amount of absolute ethanol, stir evenly, then centrifuge, finally collect the precipitate, freeze-dry to obtain the asparagine polysaccharide.
天门冬多糖的测定及结果Determination and Results of Asparagine Polysaccharide
采用苯酚-硫酸法测定上述实施例所得天门冬多糖含量,其中,粗多糖提取率按如下公式计算:Adopt the phenol-sulfuric acid method to measure the Asparagus polysaccharide content obtained in above-mentioned embodiment, wherein, crude polysaccharide extraction rate is calculated according to the following formula:
粗多糖提取率=粗多糖质量/天门冬饮片质量×100%。Extraction rate of crude polysaccharide = mass of crude polysaccharide / mass of asparagus decoction pieces × 100%.
测定结果列表如下:The test results are listed as follows:
可见,采用醇碱法提取和生产天门冬多糖,显著地提高了粗多糖提取率和总糖含量,为今后规模化生产天门冬多糖提供了很好的工艺路线,可有效保证鸡的疫苗免疫增强剂的市场供应。It can be seen that the extraction and production of asparagus polysaccharides by alcohol-alkali method has significantly improved the extraction rate of crude polysaccharides and the total sugar content, which provides a good process route for the large-scale production of asparagus polysaccharides in the future, and can effectively ensure the immune enhancement of chicken vaccines market supply of agents.
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Cited By (3)
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CN103143012A (en) * | 2013-03-26 | 2013-06-12 | 广西大学 | Traditional Chinese medicine composition and applications in preparation of porcine pseudorabies vaccine immunopotentiator |
CN110140812A (en) * | 2019-06-03 | 2019-08-20 | 广西大学 | Compound Chinese herbal medicine immune enhancer for prawns and preparation method thereof |
CN114343079A (en) * | 2021-12-20 | 2022-04-15 | 广西大学 | Anti-nitrite stress Chinese herbal medicine feed additive for Penaeus vannamei and preparation method thereof |
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CN1557842A (en) * | 2004-02-02 | 2004-12-29 | 中南大学湘雅二医院 | Extraction method, pharmaceutical preparation preparation method and application of polygonatum polysaccharide |
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CN1557842A (en) * | 2004-02-02 | 2004-12-29 | 中南大学湘雅二医院 | Extraction method, pharmaceutical preparation preparation method and application of polygonatum polysaccharide |
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《中成药》 20080620 范荣军等 五味子多糖提取工艺的比较研究 , 第06期 2 * |
《吉林大学学报(理学版)》 20060730 田洛等 醇碱提取法提取黄芪多糖 , 第04期 2 * |
《沈阳药科大学学报》 19900720 杜旭华等 抗癌植物药的开发研究__Ⅳ.中药天冬的多糖类抗癌活性成分的提取与分离 , 第03期 2 * |
Cited By (4)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103143012A (en) * | 2013-03-26 | 2013-06-12 | 广西大学 | Traditional Chinese medicine composition and applications in preparation of porcine pseudorabies vaccine immunopotentiator |
CN103143012B (en) * | 2013-03-26 | 2015-06-10 | 广西大学 | Traditional Chinese medicine composition and applications in preparation of porcine pseudorabies vaccine immunopotentiator |
CN110140812A (en) * | 2019-06-03 | 2019-08-20 | 广西大学 | Compound Chinese herbal medicine immune enhancer for prawns and preparation method thereof |
CN114343079A (en) * | 2021-12-20 | 2022-04-15 | 广西大学 | Anti-nitrite stress Chinese herbal medicine feed additive for Penaeus vannamei and preparation method thereof |
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