CN1680388A青蒿素的提取方法｜Extraction of artemisine
Entry posted by Roger in Artemisinin Patent｜青蒿素专利
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本发明公开一种提取青蒿素的方法，包括采用60～70％的乙醇为溶剂浸提原料青蒿叶，还包括：1)沉淀：调节浸提液pH值到7.5～8.0，使大部分杂质沉淀，过滤并调节母液pH值6.5～7.0；2)减压浓缩：将母液浓缩至原体积的8～1 5％，冷却除杂；3)结晶：加等量70％乙醇加热至溶解，静置析出粗结晶；4)重结晶：用热石油醚溶解粗结晶，静置分离后，得到精品。本发明采用生石灰粉CaO作为沉淀剂，既沉淀了大部分杂质，又易于结晶的形成，同时降低了成本，并采用石油醚作为的重结晶溶剂，重结晶效果优于酒精，利用本发明得到青蒿素精品总收率大于0.4％。
青蒿素的提取方法
技术领域：
本发明涉及一种中药提取方法，特别涉及从菊科植物青蒿中提取青蒿素的方法。
背景技术：
青蒿素是我国科学家在1971年首次从菊科植物黄花蒿(Artemisiaannua Linn)提取出的具有新型结构的倍半萜内酯。纯青蒿素为无色针状晶体，熔点150～153℃，比旋光度[α]D 23+75°至+78°(无水乙醇)，味苦，易溶于苯、氯仿、乙酸乙酯、丙酮和冰醋酸，能溶于乙醇、甲醇、乙醚和热石油醚。青蒿素由于具有过氧桥和缩醛结构，对酸碱不稳定，对强碱极不稳定，热至熔点以上即迅速分解。它具有十分优良的抗疟作用，包括那些对氯喹有耐药性的恶性疟原虫感染。青蒿素又是我国唯一按照西药标准研发的中药，是当前公认的治疗疟疾最有效、最安全的药物，被世界卫生组织称为“治疗疟疾的最大希望”。
目前青蒿素的提取方法如云南药物研究所的“容积汽油法”，此法简练，工艺流程短，操作方便，但收率不理想，小试仅为0.3％，工业生产≤0.2％，且大量消耗汽油，不甚安全；山东中药研究所的“丙酮—硅胶柱层析法”(专利申请号87101346A)和“低沸汽油—超短粗型球状扩孔硅胶过滤柱层析法”(专利申请号89103384)，四川省中药研究所的“稀醇法”以及美国专利(专利号4952603)“己烷提取—己烷/乙晴分析—硅胶柱层析法”，这些方法各有利弊，但工业运用都有很大的难度；云南省药物研究所另一发明“青蒿素的提取方法”(专利申请号93102934.1)中又论述，使用稀乙醇提取青蒿素，汽油萃取，活性炭脱色，用乙醇重结晶，该法在以往的工作基础上有了很大的提高，但该专利只采用一次浸泡，青蒿素不能充分溶出；使用大量汽油提取，操作危险性较大；使用活性炭脱色，不可避免地吸收部分青蒿素，降低了收率，且活性炭价格高；用50％乙醇重结晶，溶解温度高，易破坏青蒿素，效果仍不理想。
发明内容：
本法明旨在克服以上不足而提供一种提取青蒿素的方法，该方法工艺简单、产品纯度高，具有操作易掌握、溶剂消耗少、成本低、收率高、安全、不需要大型及特殊设备等优点。
为实现本发明所采取的技术方案为：
一种提取青蒿素的方法，包括采用60～70％的乙醇为溶剂浸提原料青蒿叶，还包括：
1)沉淀：调节浸提液PH值到7.5～8.0，使大部分杂质沉淀，过滤并调节母液PH值6.5～7.0；
2)减压浓缩：将母液浓缩至原体积的8～15％，冷却除杂；
3)结晶：加等量70％乙醇加热至溶解，静置析出粗结晶；
4)重结晶：用热石油醚溶解粗结晶，静置分离后，得到精品。
为了提高产品收率，采用60～70％的乙醇为溶剂浸提时，浸提次数为3～5次。
在沉淀过程中，为了降低成本和最大限度的去除杂质，调节浸提液PH值的物料为生石灰。
在沉淀过程中，为了保持青蒿素的稳定，调节母液PH值的物料为乙酸。
在浓缩过程中，为保持青蒿素稳定性，采用浓缩温度50℃～60℃，浓缩压力0.047～0.053Mpa。
在结晶过程中，为提高产品的总收率，结晶母液用再3倍量的60～70％乙醇稀释，然后重复1)、2)、3)步骤，得到粗结晶。
在重结晶过程中，利用青蒿素在冷热石油醚中溶解度差异大特性，得到更多的产品，并避免青蒿素被高温破坏，故采用沸程30～60℃的热石油醚。
本发明的积极效果为：
1、本发明经过多次浸提，最终产品的总收率相对于青蒿叶计，可达0.48％以上。
2、本发明采用酒精作为浸提溶剂，而不用汽油，大大降低了操作的风险。
3、本发明采用生石灰粉(CaO)作为沉淀剂，用CaO粉调节PH值，既沉淀了大部分杂质，又易于结晶的形成，同时降低了成本。
4、本发明采用沸程30～60℃石油醚作为的重结晶溶剂，重结晶效果优于酒精。
5、本发明浸提所用溶剂在浓缩时进行了回收，整个生产过程是在密闭状态下进行，溶剂挥发极少；浸提完成后，用水蒸汽蒸馏的方法回收酒精，残渣用作蚊香原料，这样就降低了损耗和操作风险，提高了经济效益。
具体实施方式：
实施例一：
1、浸提：将100kg青蒿叶置于中药提取罐中，加入500kg70％乙醇，开始搅拌，以10～15rpm的速度搅拌10小时，停止搅拌，使物料的大小达到60～70目，打开提取罐下部的阀门，浸提液自动沥出，得到I浸液288kg，待用；关闭阀门，再向提取罐加入300kg70％乙醇，搅拌5小时，得到II浸液313kg，待用；最后加入300kg70％乙醇，搅拌3小时，形成III浸液316kg，III浸液用于下批套用。沥干后的残渣送至酒精回收罐中，加入纯化水300kg，采用水蒸汽蒸馏法将剩余乙醇回收再利用，得到酒精(折100％)138kg，残渣用作蚊香的原料。
2、沉淀：合并I、II浸提液601kg，用生石灰粉CaO调节PH值到7.8，使大部分杂质沉淀，并迅速过滤，得到滤液，滤液用乙酸调节溶液PH值到6.7。
3、减压浓缩：将滤液转入浓缩罐中，控制减压过程中，温度保持在50℃～60℃，压力保持在0.047～0.053MPa之间，2小时内浓缩至60kg。放置冷却，倾去上清液，除去水溶性杂质，得到浓缩液11kg。
4、结晶：将浓缩液转入结晶罐中，加11kg70％乙醇加热至60℃溶解，静置3～4天，析出并收集粗结晶I0.48kg。母液用63kg70％乙醇稀释，然后按照2、3、4步骤进行沉淀，滤液减压浓缩，浓缩液结晶，收集得到粗结晶II0.13kg。合并I、II两次粗结晶得到粗结晶III0.61kg。
5、重结晶：加入1.7kg沸程为30～60℃的热石油醚溶解粗结晶III，静置24小时，析出针状结晶体，经离心分离，50～60℃真空干燥，即得到青蒿素精品482g，测定其含量，含C15H22O5 99.3％。
实施例二：
1、浸提：将100kg青蒿叶置于中药提取罐中，加入500kg60％乙醇，开始搅拌，以10～15rpm的速度搅拌10小时，停止搅拌，使物料的大小达到60～70目，打开提取罐下部的阀门，浸提液自动沥出，得到I浸液285kg，待用；关闭阀门，再向提取罐加入300kg60％乙醇，搅拌5小时，得到II浸液314kg，待用；最后加入300kg60％乙醇，搅拌3小时，得到III浸液306kg，III浸液用于下批套用。沥干后的残渣送至酒精回收罐中，加入300kg纯化水，采用水蒸汽蒸馏法将剩余乙醇回收再利用，得到酒精(折100％)122kg，残渣用作蚊香的原料。
2、沉淀：合并I、II浸提液599kg，用生石灰粉CaO调节PH值到8.0，使大部分杂质沉淀，并迅速过滤，得到滤液，滤液用乙酸调节溶液PH值到6.9。
3、减压浓缩：将滤液转入浓缩罐中，控制减压过程中，温度保持在50℃～60℃，压力保持在0.047～0.053MPa之间，2小时内浓缩至48kg。放置冷却，倾去上清液，除去水溶性杂质，得到浓缩液10.3kg。
4、结晶：将浓缩液转入结晶罐中，加10.3kg70％乙醇加热至60℃溶解，静置3～4天，析出并收集粗结晶I0.41kg。母液用60kg70％乙醇稀释，然后按照2、3、4步骤进行沉淀，滤液减压浓缩，浓缩液结晶，收集得到粗结晶II0.10kg。合并I、II两次粗结晶得到粗结晶III0.51kg。
5、重结晶：加入1.4kg沸程为30～60℃的热石油醚溶解粗结晶III，静置24小时，析出针状结晶体，经离心分离，50～60℃真空干燥，即得到青蒿素精品489g，测定其含量，含C15H22O5 99.2％。
实施例三：
1、浸提：将100kg青蒿叶置于中药提取罐中，加入500kg60％乙醇，开始搅拌，以10～15rpm的速度搅拌10小时，停止搅拌，使物料的大小达到60～70目，打开提取罐下部的阀门，浸提液自动沥出，得到I浸液283kg，待用；关闭阀门，再向提取罐加入300kg60％乙醇，搅拌5小时，得到II浸液316kg，待用；最后加入300kg60％乙醇，搅拌3小时，得到III浸液305kg，III浸液用于下批套用。沥干后的残渣送至酒精回收罐中，加入300kg纯化水，采用水蒸汽蒸馏法将剩余乙醇回收再利用，得到酒精(折100％)123kg，残渣用作蚊香的原料。
2、沉淀：合并I、II浸提液599kg，用生石灰粉CaO调节PH值到7.8，使大部分杂质沉淀，并迅速过滤，得到滤液，滤液用乙酸调节溶液PH值到6.7。
3、减压浓缩：将滤液转入浓缩罐中，控制减压过程中，温度保持在50℃～60℃，压力保持在0.047～0.053MPa之间，2小时内浓缩至60kg。放置冷却，倾去上清液，除去水溶性杂质，得到浓缩液10kg。
4、结晶：将浓缩液转入结晶罐中，加10kg70％乙醇加热至60℃溶解，静置3～4天，析出并收集粗结晶I0.43kg。母液用58.5kg60％乙醇稀释，然后按照2、3、4步骤进行沉淀，滤液减压浓缩，浓缩液结晶，收集得到粗结晶II0.11kg。合并I、II两次粗结晶得到粗结晶III0.54kg。
5、重结晶：加入1.5kg沸程为30～60℃的热石油醚溶解粗结晶III，静置24小时，析出针状结晶体，经离心分离，50～60℃真空干燥，即得到青蒿素精品483g，测定其含量，含C15H22O5 99.9％。
实施例四：
1、浸提：将100kg青蒿叶置于中药提取罐中，加入500kg60％乙醇，开始搅拌，以10～15rpm的速度搅拌10小时，停止搅拌，使物料的大小达到60～70目，打开提取罐下部的阀门，浸提液自动沥出，得到I浸液284kg，待用；关闭阀门，再向提取罐加入300kg60％乙醇，搅拌5小时，得到II浸液317kg，待用；最后加入300kg60％乙醇，搅拌3小时，得到III浸液304kg，III浸液用于下批套用。沥干后的残渣送至酒精回收罐中，加入300kg纯化水，采用水蒸汽蒸馏法将剩余乙醇回收再利用，得到酒精(折100％)123kg，残渣用作蚊香的原料。
2、沉淀：合并I、II浸提液601kg，用生石灰粉CaO调节PH值到7.5，使大部分杂质沉淀，并迅速过滤，得到滤液，滤液用乙酸调节溶液PH值到6.9。
3、减压浓缩：将滤液转入浓缩罐中，控制减压过程中，温度保持在50℃～60℃，压力保持在0.047～0.053MPa之间，2小时内浓缩至58kg。放置冷却，倾去上清液，除去水溶性杂质，得到浓缩液9.6kg。
4、结晶：将浓缩液转入结晶罐中，加9.6kg70％乙醇加热至60℃溶解，静置3～4天，析出并收集粗结晶I0.41kg。母液用56kg60％乙醇稀释，然后按照2、3、4步骤进行沉淀，滤液减压浓缩，浓缩液结晶，收集得到粗结晶II0.12kg。合并I、II两次粗结晶得到粗结晶III0.53kg。
5、重结晶：加入1.4kg沸程为30～60℃的热石油醚溶解粗结晶III，静置24小时，析出针状结晶体，经离心分离，50～60℃真空干燥，即得到青蒿素精品485g，测定其含量，含C15H22O5 99.5％。
总结：
1、一种提取青蒿素的方法，包括采用60～70％的乙醇为溶剂浸提原料青蒿叶，其特征在于还包括：
1)沉淀：调节浸提液PH值到7.5～8.0，使大部分杂质沉淀，过滤并调节母液PH值6.5～7.0；
2)减压浓缩：将母液浓缩至原体积的8～15％，冷却除杂；
3)结晶：加等量70％乙醇加热至溶解，静置析出粗结晶；
4)重结晶：用热石油醚溶解粗结晶，静置分离后，得到精品。
2、如权利要求1所述的提取青蒿素的方法，其特征在于：所述的浸提次数为3～5次。
3、如权利要求1所述的提取青蒿素的方法，其特征在于：所述调节浸提液PH值的物料为生石灰。
4、如权利要求1或3所述的提取青蒿素的方法，其特征在于：所述调节母液PH值的物料为乙酸。
5、如权利要求1所述的提取青蒿素的方法，其特征在于：所述的浓缩温度为50℃～60℃，压力为0.047～0.053MPa。
6、如权利要求1所述的提取青蒿素的方法，其特征在于：所述的结晶母液用再3倍量的60～70％乙醇稀释，然后重复1)、2)、3)步骤，得到粗结晶。
7、如权利要求1所述的提取青蒿素的方法，其特征在于：所述的石油醚为沸程30～60℃的热石油醚。
https://patents.google.com/patent/CN1680388A/zh
An extraction of qinghaosu is carried out by: 1) immersing extracting the leaf of sweet wormwood with 60-70% alcohol as solvent, depositing, regulating pH of immersing extracting liquid to 7.5-8.0, depositing the impurities, filtering, and regulating pH of mother liquid to 6.5-7.0; 2) de-pressuring and concentrating the mother liquid to 8-15% of original volume, cooling, and removing impurities; 3)crystallizing, adding into isosteric 70% alcohol, heating, dissolving, laying aside, precipitating out coarse crystal; 4)re-crystallizing, dissolving the coarse crystal by hot mineral ether, laying aside, separating, and obtaining the refined products. Its advantages include low cost, good re-crystallizing effect, and high productivity.
The extracting method of Artemisinin
Technical field:
The present invention relates to a kind of traditional Chinese medicine extraction method, particularly from the feverfew sweet wormwood, extract the method for Artemisinin.
Background technology:
Artemisinin is the sesquiterpene lactones with novel texture that China scientist extracted from feverfew Herba Artemisiae annuae (Artemisiaannua Linn) first in 1971.Pure Artemisinin is a colourless acicular crystal, 150～153 ℃ of fusing points, specific rotatory power [α] D 23+ 75 ° to+78 ° (dehydrated alcohol), bitter is soluble in benzene, chloroform, ethyl acetate, acetone and Glacial acetic acid, can be dissolved in ethanol, methyl alcohol, ether and hot sherwood oil.Artemisinin is owing to have peroxide bridge and ethylidene ether structure, and extremely unstable to highly basic to the soda acid instability, heat is to promptly decomposing rapidly more than the fusing point.It has very good antimalarial effect, comprises that those have chemical sproof falciparum infection to chloroquine.Artemisinin is again the unique Chinese medicine according to the research and development of Western medicine standard of China, is current generally acknowledged the most effective, the safest medicine of treatment malaria, is called " maximum of treatment malaria is wished " by the World Health Organization.
The extracting method of present Artemisinin such as " the volume gasoline method " of institute of materia medica, Yunnan, this method is terse, and technical process is short, and is easy to operate, but yield is undesirable, and lab scale only is 0.3%, and industrial production≤0.2%, and mass consumption gasoline are unsafe; " acetone-silica gel column chromatography " of institute of Chinese materia medica, Shandong (number of patent application 87101346A) and " the low spherical reaming filtered through silica gel of the gasoline-super short-thick type column chromatography that boils " (number of patent application 89103384), " rare pure method " of Traditional Chinese Medicine Research Institute, Sichuan Province and United States Patent (USP) (patent No. 4952603) " the fine analysis-silica gel column chromatography of hexane extraction-hexane/second ", these methods cut both ways, but industrial applicability all has very big difficulty; Discuss again in another invention " extracting method of Artemisinin " (number of patent application 93102934.1) of Yunnan Pharmaceutical Institute, use Diluted Alcohol to extract Artemisinin, gasoline extraction, activated carbon decolorizing, use ethyl alcohol recrystallization, this method is greatly improved on working foundation in the past, but this patent only adopts once immersion, fully stripping of Artemisinin; Use a large amount of gasoline extraction, operational danger is bigger; Use activated carbon decolorizing, the absorption portion Artemisinin has reduced yield inevitably, and gac price height; Use 50% ethyl alcohol recrystallization, the solvent temperature height, the destructible Artemisinin, effect is still undesirable.
Summary of the invention:
This law is bright to be intended to overcome above deficiency and a kind of method of extracting Artemisinin is provided, and this method technology is simple, product purity is high, have that operation is easily grasped, solvent consumption is few, cost is low, yield is high, safe, do not need large-scale and advantage such as specific installation.
For realizing that the technical solution used in the present invention is:
A kind of method of extracting Artemisinin comprises that the ethanol of employing 60～70% is solvent lixiviate raw material artemisia leaf, also comprises:
1) precipitation: regulate vat liquor pH value to 7.5～8.0, make most of contamination precipitation, filter and regulate mother liquor pH value 6.5～7.0;
2) concentrating under reduced pressure: mother liquor is concentrated into 8～15% of original volume, the cooling removal of impurities;
3) crystallization: add equivalent 70% ethanol and be heated to dissolving, leave standstill and separate out coarse crystallization;
4) recrystallization:, after the standing separation, obtain elaboration with hot petroleum ether dissolution coarse crystallization.
In order to improve product yield, when the ethanol of employing 60～70% was the solvent lixiviate, the lixiviate number of times was 3～5 times.
In precipitation process, in order to reduce cost and to remove impurity to greatest extent, the material of regulating the vat liquor pH value is a unslaked lime.
In precipitation process, in order to keep the stable of Artemisinin, the material of regulating the mother liquor pH value is an acetate.
In concentration process, for keeping Artemisinin stability, adopt 50 ℃～60 ℃ of thickening temperatures, concentrate pressure 0.047～0.053Mpa.
In crystallisation process, be to improve the total recovery of product, crystalline mother solution repeats 1 then with 60～70% alcohol dilutions of 3 times of amounts again), 2), 3) step, obtain coarse crystallization.
In recrystallization process, utilize Artemisinin big characteristic of dissolubility difference in cold and hot sherwood oil, obtain more products, and avoid Artemisinin to be destroyed, so adopt the hot sherwood oil of 30～60 ℃ of boiling ranges by high temperature.
Positively effect of the present invention is:
1, the present invention is through extracted many times, and the total recovery of the finished product can reach more than 0.48% with respect to the artemisia leaf meter.
2, the present invention adopts alcohol as extraction solvent, and without gasoline, greatly reduces the risk of operation.
3, the present invention adopts calcium lime powder (CaO) as precipitation agent, regulates pH value with the CaO powder, has both precipitated most of impurity, is easy to crystalline again and forms, and has reduced cost simultaneously.
4, the present invention adopts the recrystallization solvent of 30～60 ℃ of sherwood oil conducts of boiling range, and the recrystallization effect is better than alcohol.
5, lixiviate solvent for use of the present invention reclaims when concentrated, and whole process of production is to carry out under air-tight state, and solvent evaporates is few; After lixiviate is finished, the steam distilled method recovered alcohol of water, residue has so just reduced loss and operational risk as the mosquito-repellent incense raw material, has improved economic benefit.
Embodiment:
Embodiment one:
1, lixiviate: the 100kg artemisia leaf is placed the traditional Chinese medicine extraction jar, add 500kg70% ethanol, begin to stir, speed with 10～15rpm stirred 10 hours, stopped to stir, and made the size of material reach 60～70 orders, open the valve of extractor bottom, the automatic drop of vat liquor goes out, and obtains I immersion liquid 288kg, and is stand-by; Valve-off adds 300kg70% ethanol to extractor again, stirs 5 hours, obtains II immersion liquid 313kg, and is stand-by; Add 300kg70% ethanol at last, stirred 3 hours, form III immersion liquid 316kg, the III immersion liquid is used for following batch and applies mechanically.Residue after draining is delivered in the alcohol withdrawing can, adds purified water 300kg, adopts steam distillation will remain the ethanol recycling, obtains alcohol (folding 100%) 138kg, and residue is as the raw material of mosquito-repellent incense.
2, precipitation: merging I, II vat liquor 601kg, regulate pH value to 7.8 with calcium lime powder CaO, make most of contamination precipitation, and filter rapidly, obtain filtrate, filtrate is used acetate regulator solution pH value to 6.7.
3, concentrating under reduced pressure: filtrate is changed in the concentration tank, and in the control decompression process, temperature remains on 50 ℃～60 ℃, and pressure remains between 0.047～0.053MPa, is concentrated into 60kg in 2 hours.Place cooling, the supernatant liquor that inclines is removed water-soluble impurity, obtains concentrated solution 11kg.
4, crystallization: concentrated solution is changed in the crystallizer, add 11kg70% ethanol and be heated to 60 ℃ of dissolvings, left standstill 3～4 days, separate out and collect coarse crystallization I0.48kg.Mother liquor 63kg70% alcohol dilution precipitates according to 2,3,4 steps then, and filtrate decompression concentrates, and the concentrated solution crystallization is collected and obtained coarse crystallization II0.13kg.Merge twice coarse crystallization of I, II and obtain coarse crystallization III0.61kg.
5, recrystallization: adding 1.7kg boiling range is 30～60 ℃ hot petroleum ether dissolution coarse crystallization III, leaves standstill 24 hours, separates out acicular crystals, and through centrifugation, 50～60 ℃ of vacuum-dryings promptly obtain Artemisinin elaboration 482g, measure its content, contain C 15H 22O 599.3%.
Embodiment two:
1, lixiviate: the 100kg artemisia leaf is placed the traditional Chinese medicine extraction jar, add 500kg60% ethanol, begin to stir, speed with 10～15rpm stirred 10 hours, stopped to stir, and made the size of material reach 60～70 orders, open the valve of extractor bottom, the automatic drop of vat liquor goes out, and obtains I immersion liquid 285kg, and is stand-by; Valve-off adds 300kg60% ethanol to extractor again, stirs 5 hours, obtains II immersion liquid 314kg, and is stand-by; Add 300kg60% ethanol at last, stirred 3 hours, obtain III immersion liquid 306kg, the III immersion liquid is used for following batch and applies mechanically.Residue after draining is delivered in the alcohol withdrawing can, adds the 300kg purified water, adopts steam distillation will remain the ethanol recycling, obtains alcohol (folding 100%) 122kg, and residue is as the raw material of mosquito-repellent incense.
2, precipitation: merging I, II vat liquor 599kg, regulate pH value to 8.0 with calcium lime powder CaO, make most of contamination precipitation, and filter rapidly, obtain filtrate, filtrate is used acetate regulator solution pH value to 6.9.
3, concentrating under reduced pressure: filtrate is changed in the concentration tank, and in the control decompression process, temperature remains on 50 ℃～60 ℃, and pressure remains between 0.047～0.053MPa, is concentrated into 48kg in 2 hours.Place cooling, the supernatant liquor that inclines is removed water-soluble impurity, obtains concentrated solution 10.3kg.
4, crystallization: concentrated solution is changed in the crystallizer, add 10.3kg70% ethanol and be heated to 60 ℃ of dissolvings, left standstill 3～4 days, separate out and collect coarse crystallization I0.41kg.Mother liquor 60kg70% alcohol dilution precipitates according to 2,3,4 steps then, and filtrate decompression concentrates, and the concentrated solution crystallization is collected and obtained coarse crystallization II0.10kg.Merge twice coarse crystallization of I, II and obtain coarse crystallization III0.51kg.
5, recrystallization: adding 1.4kg boiling range is 30～60 ℃ hot petroleum ether dissolution coarse crystallization III, leaves standstill 24 hours, separates out acicular crystals, and through centrifugation, 50～60 ℃ of vacuum-dryings promptly obtain Artemisinin elaboration 489g, measure its content, contain C 15H 22O 599.2%.
Embodiment three:
1, lixiviate: the 100kg artemisia leaf is placed the traditional Chinese medicine extraction jar, add 500kg60% ethanol, begin to stir, speed with 10～15rpm stirred 10 hours, stopped to stir, and made the size of material reach 60～70 orders, open the valve of extractor bottom, the automatic drop of vat liquor goes out, and obtains I immersion liquid 283kg, and is stand-by; Valve-off adds 300kg60% ethanol to extractor again, stirs 5 hours, obtains II immersion liquid 316kg, and is stand-by; Add 300kg60% ethanol at last, stirred 3 hours, obtain III immersion liquid 305kg, the III immersion liquid is used for following batch and applies mechanically.Residue after draining is delivered in the alcohol withdrawing can, adds the 300kg purified water, adopts steam distillation will remain the ethanol recycling, obtains alcohol (folding 100%) 123kg, and residue is as the raw material of mosquito-repellent incense.
2, precipitation: merging I, II vat liquor 599kg, regulate pH value to 7.8 with calcium lime powder CaO, make most of contamination precipitation, and filter rapidly, obtain filtrate, filtrate is used acetate regulator solution pH value to 6.7.
3, concentrating under reduced pressure: filtrate is changed in the concentration tank, and in the control decompression process, temperature remains on 50 ℃～60 ℃, and pressure remains between 0.047～0.053MPa, is concentrated into 60kg in 2 hours.Place cooling, the supernatant liquor that inclines is removed water-soluble impurity, obtains concentrated solution 10kg.
4, crystallization: concentrated solution is changed in the crystallizer, add 10kg70% ethanol and be heated to 60 ℃ of dissolvings, left standstill 3～4 days, separate out and collect coarse crystallization I0.43kg.Mother liquor 58.5kg60% alcohol dilution precipitates according to 2,3,4 steps then, and filtrate decompression concentrates, and the concentrated solution crystallization is collected and obtained coarse crystallization II0.11kg.Merge twice coarse crystallization of I, II and obtain coarse crystallization III0.54kg.
5, recrystallization: adding 1.5kg boiling range is 30～60 ℃ hot petroleum ether dissolution coarse crystallization III, leaves standstill 24 hours, separates out acicular crystals, and through centrifugation, 50～60 ℃ of vacuum-dryings promptly obtain Artemisinin elaboration 483g, measure its content, contain C 15H 22O 599.9%.
Embodiment four:
1, lixiviate: the 100kg artemisia leaf is placed the traditional Chinese medicine extraction jar, add 500kg60% ethanol, begin to stir, speed with 10～15rpm stirred 10 hours, stopped to stir, and made the size of material reach 60～70 orders, open the valve of extractor bottom, the automatic drop of vat liquor goes out, and obtains I immersion liquid 284kg, and is stand-by; Valve-off adds 300kg60% ethanol to extractor again, stirs 5 hours, obtains II immersion liquid 317kg, and is stand-by; Add 300kg60% ethanol at last, stirred 3 hours, obtain III immersion liquid 304kg, the III immersion liquid is used for following batch and applies mechanically.Residue after draining is delivered in the alcohol withdrawing can, adds the 300kg purified water, adopts steam distillation will remain the ethanol recycling, obtains alcohol (folding 100%) 123kg, and residue is as the raw material of mosquito-repellent incense.
2, precipitation: merging I, II vat liquor 601kg, regulate pH value to 7.5 with calcium lime powder CaO, make most of contamination precipitation, and filter rapidly, obtain filtrate, filtrate is used acetate regulator solution pH value to 6.9.
3, concentrating under reduced pressure: filtrate is changed in the concentration tank, and in the control decompression process, temperature remains on 50 ℃～60 ℃, and pressure remains between 0.047～0.053MPa, is concentrated into 58kg in 2 hours.Place cooling, the supernatant liquor that inclines is removed water-soluble impurity, obtains concentrated solution 9.6kg.
4, crystallization: concentrated solution is changed in the crystallizer, add 9.6kg70% ethanol and be heated to 60 ℃ of dissolvings, left standstill 3～4 days, separate out and collect coarse crystallization I0.41kg.Mother liquor 56kg60% alcohol dilution precipitates according to 2,3,4 steps then, and filtrate decompression concentrates, and the concentrated solution crystallization is collected and obtained coarse crystallization II0.12kg.Merge twice coarse crystallization of I, II and obtain coarse crystallization III0.53kg.
5, recrystallization: adding 1.4kg boiling range is 30～60 ℃ hot petroleum ether dissolution coarse crystallization III, leaves standstill 24 hours, separates out acicular crystals, and through centrifugation, 50～60 ℃ of vacuum-dryings promptly obtain Artemisinin elaboration 485g, measure its content, contain C 15H 22O 599.5%.
1, a kind of method of extracting Artemisinin comprises that the ethanol of employing 60～70% is solvent lixiviate raw material artemisia leaf, it is characterized in that also comprising:
1) precipitation: regulate vat liquor pH value to 7.5～8.0, make most of contamination precipitation, filter and regulate mother liquor pH value 6.5～7.0;
2) concentrating under reduced pressure: mother liquor is concentrated into 8～15% of original volume, the cooling removal of impurities;
3) crystallization: add equivalent 70% ethanol and be heated to dissolving, leave standstill and separate out coarse crystallization;
4) recrystallization:, after the standing separation, obtain elaboration with hot petroleum ether dissolution coarse crystallization.
2, the method for extraction Artemisinin as claimed in claim 1 is characterized in that: described lixiviate number of times is 3～5 times.
3, the method for extraction Artemisinin as claimed in claim 1 is characterized in that: the material of described adjusting vat liquor pH value is a unslaked lime.
4, as the method for claim 1 or 3 described extraction Artemisinins, it is characterized in that: the material of described adjusting mother liquor pH value is an acetate.
5, the method for extraction Artemisinin as claimed in claim 1 is characterized in that: described thickening temperature is 50 ℃～60 ℃, and pressure is 0.047～0.053MPa.
6, the method for extraction Artemisinin as claimed in claim 1 is characterized in that: described crystalline mother solution repeats 1 then with 60～70% alcohol dilutions of 3 times of amounts again), 2), 3) step, obtain coarse crystallization.
7, the method for extraction Artemisinin as claimed in claim 1 is characterized in that: described sherwood oil is the hot sherwood oil of 30～60 ℃ of boiling ranges.
https://patents.google.com/patent/CN1680388A/en
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