CN1660172A - A new anti-hepatitis B virus drug and its preparation process - Google Patents
- ️Wed Aug 31 2005
CN1660172A - A new anti-hepatitis B virus drug and its preparation process - Google Patents
A new anti-hepatitis B virus drug and its preparation process Download PDFInfo
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Publication number
- CN1660172A CN1660172A CN2004100219458A CN200410021945A CN1660172A CN 1660172 A CN1660172 A CN 1660172A CN 2004100219458 A CN2004100219458 A CN 2004100219458A CN 200410021945 A CN200410021945 A CN 200410021945A CN 1660172 A CN1660172 A CN 1660172A Authority
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- China Prior art keywords
- ethanol
- leaching
- solution
- reflux
- hepatitis Prior art date
- 2004-02-23 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.)
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- 238000002360 preparation method Methods 0.000 title claims description 5
- 229940124405 anti-hepatitis b virus drug Drugs 0.000 title claims description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 51
- 238000010992 reflux Methods 0.000 claims abstract description 12
- 208000002672 hepatitis B Diseases 0.000 claims abstract description 11
- 241001629511 Litchi Species 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 8
- 229920005989 resin Polymers 0.000 claims abstract description 8
- 238000001179 sorption measurement Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 20
- 238000002386 leaching Methods 0.000 claims description 18
- 238000000605 extraction Methods 0.000 claims description 8
- 239000002547 new drug Substances 0.000 claims description 6
- 244000183278 Nephelium litchi Species 0.000 claims description 5
- 235000015742 Nephelium litchi Nutrition 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 4
- 239000007864 aqueous solution Substances 0.000 claims description 3
- 241000143437 Aciculosporium take Species 0.000 claims description 2
- 241000701076 Macacine alphaherpesvirus 1 Species 0.000 claims description 2
- 239000002156 adsorbate Substances 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 238000001816 cooling Methods 0.000 claims description 2
- 238000004821 distillation Methods 0.000 claims description 2
- 229940126534 drug product Drugs 0.000 claims description 2
- 239000003480 eluent Substances 0.000 claims description 2
- 239000000843 powder Substances 0.000 claims description 2
- 239000012141 concentrate Substances 0.000 claims 2
- 239000003814 drug Substances 0.000 abstract description 9
- 238000005406 washing Methods 0.000 abstract 2
- 239000007788 liquid Substances 0.000 abstract 1
- 238000010298 pulverizing process Methods 0.000 abstract 1
- 229940079593 drug Drugs 0.000 description 7
- 241000700721 Hepatitis B virus Species 0.000 description 4
- 208000000419 Chronic Hepatitis B Diseases 0.000 description 2
- 208000015181 infectious disease Diseases 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 208000035473 Communicable disease Diseases 0.000 description 1
- 108090000695 Cytokines Proteins 0.000 description 1
- 102000004127 Cytokines Human genes 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 238000012404 In vitro experiment Methods 0.000 description 1
- 102000014150 Interferons Human genes 0.000 description 1
- 108010050904 Interferons Proteins 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 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 description 1
- -1 anthraquinone compounds Chemical class 0.000 description 1
- 239000000427 antigen Substances 0.000 description 1
- 102000036639 antigens Human genes 0.000 description 1
- 108091007433 antigens Proteins 0.000 description 1
- 229940097217 cardiac glycoside Drugs 0.000 description 1
- 239000002368 cardiac glycoside Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 235000013399 edible fruits Nutrition 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 230000005764 inhibitory process Effects 0.000 description 1
- 229940079322 interferon Drugs 0.000 description 1
- 150000002596 lactones Chemical class 0.000 description 1
- 231100000053 low toxicity Toxicity 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 239000002777 nucleoside Substances 0.000 description 1
- 150000003833 nucleoside derivatives Chemical class 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000008520 organization Effects 0.000 description 1
- 239000000825 pharmaceutical preparation Substances 0.000 description 1
- 108090000765 processed proteins & peptides Proteins 0.000 description 1
- 238000001694 spray drying Methods 0.000 description 1
- 229930002534 steroid glycoside Natural products 0.000 description 1
- 150000008143 steroidal glycosides Chemical class 0.000 description 1
- 238000001291 vacuum drying Methods 0.000 description 1
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- Medicines Containing Plant Substances (AREA)
Abstract
A medicine for suppressing HBV and treating hepatitis B is prepared from litchi kernel through washing, drying in air, pulverizing, thermal reflux extracting in alcohol solution, filtering to remove dregs, recovering alcohol, adsorbing by macroreticular adsorption resin, water washing, alcohol eluting, collecting the eluting liquid, concentrating and drying.
Description
(一)技术领域：(1) Technical field:
本发明涉及从植物果核中提取出有效药物成份制备的新药，特别是一种用荔枝核制成的抗乙肝病毒的新药及其制备工艺。The invention relates to a new drug prepared by extracting effective drug components from plant fruit cores, in particular to a new drug against hepatitis B virus made from litchi cores and a preparation process thereof.
(二)背景技术：(two) background technology:
乙型肝炎(简称乙肝)是由乙型肝炎病毒(HBV)感染引发的一种常见的传染病。根据国际卫生组织(WHO)估测，全球至少有3.5亿人携带(HBV)。流行病学调查显示，我国人群乙肝表面抗原(HBSAg)检出率达10％，慢性乙肝的流行率为0.1％。目前用于治疗慢性乙肝的药物主要是干扰素、核苷类药物、以及其它细胞因子及免疫肽类药物。这些药物价格昂贵，疗效并不能令人满意，对一些患者甚至还有严重的不良反应。因此，迫切需要在天然药物中开发低毒、高效、资源富厚的乙肝治疗药。Hepatitis B (referred to as hepatitis B) is a common infectious disease caused by hepatitis B virus (HBV) infection. According to the World Health Organization (WHO) estimates, there are at least 350 million people in the world carrying (HBV). Epidemiological surveys show that the detection rate of hepatitis B surface antigen (HB SA g ) in the Chinese population is 10%, and the prevalence rate of chronic hepatitis B is 0.1%. The drugs currently used to treat chronic hepatitis B are mainly interferon, nucleoside drugs, and other cytokines and immune peptide drugs. These medicines are expensive, their efficacy is not satisfactory, and some patients even have serious adverse reactions. Therefore, there is an urgent need to develop low-toxicity, high-efficiency, and resource-rich hepatitis B therapeutics in natural medicines.
(三)发明内容：(3) Contents of the invention:
本发明的目的是要公开一种以荔枝核为原料提取出抗乙肝药用成份制作抗乙肝病毒新药及其制备工艺。The purpose of the present invention is to disclose a new anti-hepatitis B virus drug and its preparation process by extracting anti-hepatitis B medicinal components from litchi cores.
具体的技术措施是：将粉碎的荔枝核浸入乙醇中回流浸提、过滤弃渣、回收乙醇，余下的水溶液过大孔吸附树脂吸附富集、水洗至流出液无色，再用乙醇洗脱，收集洗脱液、浓缩干燥即制得新药成品。The specific technical measures are: immerse the crushed lychee core in ethanol for reflux extraction, filter the discarded residue, recover ethanol, absorb and enrich the remaining aqueous solution through a macroporous adsorption resin, wash with water until the effluent is colorless, and then elute with ethanol. The eluate is collected, concentrated and dried to obtain the finished drug.
据分析，新药中主要为黄酮类、蒽醌类化合物和有机酸、强心甙、内脂等成份，经体外实验证明，其对乙肝病毒的抑制率大于85％以上。荔枝核本属废弃物，来源广，易收集，本发明可使其变废为宝、造福人类。According to analysis, the new drug is mainly composed of flavonoids, anthraquinone compounds, organic acids, cardiac glycosides, lactones and other components. It has been proved by in vitro experiments that its inhibition rate against hepatitis B virus is more than 85%. The lychee core belongs to waste, has wide sources and is easy to collect. The invention can turn waste into treasure and benefit mankind.
(四)具体实施方案：(4) Specific implementation plan:
从荔枝核中提取抗乙肝病毒新药的制备工艺流程为：The preparation process of extracting anti-hepatitis B virus new drug from litchi core is as follows:
洗净、晾干、粉碎荔枝核——乙醇溶液加热回流提取——过滤弃渣——回收乙醇——水溶液过大孔吸附树脂吸附富集——水洗树脂柱至流出液无色——乙醇洗脱、收集洗脱液——浓缩、干燥——成品。Wash, dry, and crush litchi cores—heat reflux with ethanol solution to extract—filter and discard residue—recover ethanol—adsorb and enrich aqueous solution through macroporous adsorption resin—wash the resin column with water until the effluent is colorless—wash with ethanol Stripping and collecting the eluent—concentration, drying—the finished product.
具体工艺是：The specific process is:
a、取洗净、晾干、无腐迹的荔枝核粉碎至30～50目，置于浸提罐中；a. Take litchi cores that have been washed, dried, and free from rot, and crushed to 30-50 mesh, and placed in an extraction tank;
b、加入荔枝核粉质量6～10倍、浓度为50～70％的乙醇溶液，加热回流1.5～2小时浸取，滤出浸取液，又另加入同量的乙醇溶液，加热回流1.5～2小时，滤出浸取液，如此共重复回流浸取3次；b. Add 6 to 10 times the mass of lychee kernel powder and an ethanol solution with a concentration of 50 to 70%, heat and reflux for 1.5 to 2 hours for leaching, filter out the leaching solution, add the same amount of ethanol solution, and heat and reflux for 1.5 to 2 hours. After 2 hours, filter out the leaching solution, and repeat the reflux leaching for 3 times;
c、合并3次浸取液，置于蒸馏罐中，加热至沸腾，回收乙醇；c. Merge the leaching solutions for 3 times, place them in a distillation tank, heat to boiling, and reclaim ethanol;
d、过滤回收乙醇后的浸取液，滤除不溶物；d, filter and recover the leaching solution after ethanol, and filter out insoluble matter;
e、将滤除不溶物后的浸取液，过大孔吸附树脂，吸附完成后，用水洗树脂柱至流出液无色，再用80％的乙醇洗脱吸附物，收集洗脱液；e. Pass the leaching solution after filtering out the insoluble matter through the macroporous adsorption resin. After the adsorption is completed, wash the resin column with water until the effluent is colorless, then elute the adsorbate with 80% ethanol, and collect the eluent;
f、将洗脱液回收乙醇后，继续加热浓缩至浓缩液含固量大于60％的浸膏状；f. After recovering the ethanol from the eluate, continue heating and concentrating until the concentrated solution has a solid content greater than 60%;
g、将浸膏置于浸提罐中，加入浸膏质量6～10倍、浓度≥90％的乙醇，进行加热回流浸提，重复3次，合并3次的浸取液，冷却后，除去不溶物；g. Put the extract in the extraction tank, add 6-10 times the mass of the extract, and ethanol with a concentration ≥ 90%, carry out heating and reflux extraction, repeat 3 times, combine the leaching solution for 3 times, after cooling, remove Insolubles;
h、将浸取液加热回收乙醇，至含固量为28～35％，干燥(采用真空干燥或喷雾干燥均可)，即制得从荔枝核中提取的抗乙肝新药产品。h. Heating the leaching solution to recover ethanol until the solid content is 28-35%, and drying (vacuum drying or spray drying can be used), and the new anti-hepatitis B drug product extracted from the litchi core is obtained.
Claims (2)
1、一种抗乙肝病毒新药，其特征在于：它是将粉碎的荔枝核浸入乙醇中回流浸提、过滤弃渣、回收乙醇，余下的水溶液过大孔吸附树脂吸附富集、水洗至流出液无色，再用乙醇洗脱，收集洗脱液、浓缩干燥，制得新药成品。1. A novel anti-hepatitis B virus drug, characterized in that: it immerses pulverized lychee cores in ethanol for reflux extraction, filters and discards residues, reclaims ethanol, and the remaining aqueous solution is absorbed and enriched by a macroporous adsorption resin, washed with water until the effluent It is colorless, and then eluted with ethanol, and the eluate is collected, concentrated and dried to obtain a new drug product. 2、从荔枝核中提取的抗乙肝病毒新药的制备工艺：其特征是：2. The preparation process of the anti-hepatitis B virus new drug extracted from litchi core: it is characterized in that: a、取洗净、晾干、无腐迹的荔枝核粉碎至30～50目，置于浸提罐中；a. Take litchi cores that have been washed, dried, and free from rot, and crushed to 30-50 mesh, and placed in an extraction tank; b、加入荔枝核粉质量6～10倍、浓度为50～70％的乙醇溶液，加热回流1.5～2小时浸取，滤出浸取液，另加入同量的乙醇溶液，加热回流1.5～2小时，滤出浸取液，共重复回流浸取3次；b. Add 6 to 10 times the mass of lychee kernel powder and an ethanol solution with a concentration of 50 to 70%, heat and reflux for 1.5 to 2 hours for leaching, filter out the leaching solution, add the same amount of ethanol solution, and heat and reflux for 1.5 to 2 hours. hour, filter out the leaching solution, and repeat reflux leaching 3 times; c、合并3次浸取液，置于蒸馏罐中，加热至沸腾，回收乙醇；c. Merge the leaching solutions for 3 times, place them in a distillation tank, heat to boiling, and reclaim ethanol; d、过滤回收乙醇后的浸取液，滤除不溶物；d, filter and recover the leaching solution after ethanol, and filter out insoluble matter; e、将滤除不溶物后的浸取液澄清，过大孔吸附树脂，吸附完成后，用水洗树脂柱至流出液无色，再用80％的乙醇洗脱吸附物，收集洗脱液；e. Clarify the leaching solution after filtering out the insoluble matter, pass through the macroporous adsorption resin, after the adsorption is completed, wash the resin column with water until the effluent is colorless, then elute the adsorbate with 80% ethanol, and collect the eluent; f、将洗脱液回收乙醇后，加热浓缩至浓缩液含固量大于60％的浸膏状；f. After recovering the ethanol from the eluate, heat and concentrate until the concentrate has a solid content greater than 60%; g、将浸膏置于浸提罐中，加入浸膏质量6～10倍、浓度≥90％的乙醇，进行加热回流浸提，重复3次，合并3次的浸取液，冷却后除去不溶物；g. Put the extract in an extraction tank, add ethanol with 6 to 10 times the mass of the extract and a concentration ≥ 90%, carry out heating and reflux extraction, repeat 3 times, combine the leaching solution for 3 times, and remove the insoluble after cooling thing; h、将浸取液加热回收乙醇，至含固量为28～35％，干燥，制得成品。h. Heating the leaching solution to recover ethanol until the solid content is 28-35%, and drying to obtain a finished product.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2004100219458A CN1660172A (en) | 2004-02-23 | 2004-02-23 | A new anti-hepatitis B virus drug and its preparation process |
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| Application Number | Priority Date | Filing Date | Title |
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| CN2004100219458A CN1660172A (en) | 2004-02-23 | 2004-02-23 | A new anti-hepatitis B virus drug and its preparation process |
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Cited By (4)
* Cited by examiner, † Cited by third party| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1879743B (en) * | 2006-04-29 | 2010-05-12 | 岭南荔枝加工工程技术惠州研究中心 | Oral liquid of litchi seed and method for making same |
| CN102048885A (en) * | 2011-01-10 | 2011-05-11 | 广州市中医医院 | Extraction process for lychee seed saponin |
| CN102151306A (en) * | 2011-04-11 | 2011-08-17 | 中山大学 | Active combined product extracted from leechee pulp, preparation method thereof and application thereof |
| CN104225037A (en) * | 2014-09-22 | 2014-12-24 | 广西医科大学 | Preparation method of litchi seed extract for preventing and treating prostatic cancer and application of litchi seed extract |
-
2004
- 2004-02-23 CN CN2004100219458A patent/CN1660172A/en active Pending
Cited By (4)
* Cited by examiner, † Cited by third party| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1879743B (en) * | 2006-04-29 | 2010-05-12 | 岭南荔枝加工工程技术惠州研究中心 | Oral liquid of litchi seed and method for making same |
| CN102048885A (en) * | 2011-01-10 | 2011-05-11 | 广州市中医医院 | Extraction process for lychee seed saponin |
| CN102151306A (en) * | 2011-04-11 | 2011-08-17 | 中山大学 | Active combined product extracted from leechee pulp, preparation method thereof and application thereof |
| CN104225037A (en) * | 2014-09-22 | 2014-12-24 | 广西医科大学 | Preparation method of litchi seed extract for preventing and treating prostatic cancer and application of litchi seed extract |
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