CN100384479C - Method for preparing bile acid adsorbent of beta cyclo dextrin polymer - Google Patents
Method for preparing bile acid adsorbent of beta cyclo dextrin polymer Download PDFInfo
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- CN100384479C CN100384479C CNB200610013725XA CN200610013725A CN100384479C CN 100384479 C CN100384479 C CN 100384479C CN B200610013725X A CNB200610013725X A CN B200610013725XA CN 200610013725 A CN200610013725 A CN 200610013725A CN 100384479 C CN100384479 C CN 100384479C
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Abstract
This invention discloses a preparation method for bile acid sorbent of beta-ring dextrin polymer including: mixing beta-ring dextrin with crosslinking agent epoxy chloropropane, 1, 2 glycop twice-shrunk glyceryl ether or 1, 2-butylene-glycol twice-shrunk glyceryl ether, then dropping 37% thick HCL, 98% thick HNO3, 98% H2SO4 or perchloric acid in it to be mixed to get the bile acid sorbent of beta-ring dextrin polymer, or firstly solving the epoxy chloropropane, the 1,2-glycop twice-shrunk glyceryl ether or 1,2-butylene-glycol twi-shrunk glyceryl ether in tetrachloroethylene then solving the beta-ring dextrin solution in the tetrachloroethylene solution, then adding 37% thick HCL, 98% H2SO4 or perchloric acid in it to be reacted to get the sorbent.
Description
Technical field
The present invention relates to a kind of preparation method of bile acid adsorbent of beta cyclo dextrin polymer, belong to the bile acid adsorbent technology.
Background technology
Atherosclerosis is a kind of disease of serious harm human life health, and itself and hyperlipemia are in close relations, and hyper acid because of being in the human body bile for the hyperlipemia main diseases.Present antiatherogenic medicine is a lot, mainly based on blood lipid regulation---reduce LDL-C (LDL-C), while high density lipoprotein increasing-cholesterol (HDL-C), represent medicine as influencing the cholesterol absorption medicine, influence cholesterol and triglyceride metabolism medicine, influencing cholesterol distribution and transhipment medicine, newtype drugs such as HMG-CoA reductase inhibitor etc.; In recent years some oral adsorbents also occur and be used for reducing bile acid concentration, as ion exchange resin type bile acid chelating agent-colestyramine (cholestyramine), the hydrochloric acid colesevelam of colestipol (colestipo1) and up-to-date listing (colesevelam hydrochloride), its principle is by the exchange anionic group, in intestinal, combine with the bile salt anion, forming complex discharges with feces, the enterohepatic circulation of bile acid is interfered, promoted the conversion of cholesterol in hepatocyte, reached effect for reducing fat thereby blood plasma cholesterol level is descended.There are many untoward reaction in the fat-reducing medicament of clinical practice because medicine time is long, as gastrointestinal reaction and liver dysfunction etc., has limited the performance of curative effect.Oral adsorbent is not absorbed, and does not enter systemic circulation, and is less to liver dysfunction, but has simultaneously following shortcoming yet: 1. dosage is excessive and the ammonia stink is arranged, and makes patient be difficult to stand, and is non-critical patient especially, often is reluctant to take medicine; 2. significantly intestines and stomach side effect, as dyspepsia, constipation, feel sick, stomachache, hemorrhoid, anal fissure, hernia aggravation etc., bring difficulty to long-term prescription.
Beta-schardinger dextrin-has clathration to bile acid, conjugated bile acid, and the effects such as conversion of bile acid in small intestinal microbial activities, the acceleration bodies are regulated in the drainage of bile acid in the absorption of minimizing bile acid, the increase feces.Beta cyclo dextrin polymer has not only kept the ability of original molecule inclusion of cyclodextrin and identification, has polymer excellent mechanical intensity, stability and chemical adjustability etc. simultaneously again concurrently.Therefore reduce bile acid, the significant and wide prospect of the atherosclerotic newtype drug of treatment for developing.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of bile acid adsorbent of beta cyclo dextrin polymer, simple, the prepared adsorbent of this method preparation technology is to the bile acid high adsorption capacity, and is cheap.
The present invention is realized by following technical proposals, a kind of preparation method of beta cyclo dextrin polymer bile acid adsorbent, and method 1 its feature comprises following process:
1) with beta-schardinger dextrin-and cross-linking agent epoxychloropropane, 1,2-Ethylene glycol diglycidyl ether or 1, the solution of 2-butanediol diglycidyl ether is 1 by the ratio of quality and volume: 1-20 (g/mL), with beta-schardinger dextrin-and cross-linking agent epoxychloropropane, 1,2-Ethylene glycol diglycidyl ether or 1,2-butanediol diglycidyl ether solution mixes, be standard again with the beta-schardinger dextrin-, ratio in quality and volume is 1: the ratio of 0.1-5 (g/mL) slowly drips 37% concentrated hydrochloric acid while stirring, 98% concentrated nitric acid, 98% sulphuric acid or perchloric acid, slowly stir 10-90 ℃ of reaction 1-20h, obtain the bile acid adsorbent of beta cyclo dextrin polymer.
Method 2 its features comprise following process:
1) earlier according to 1-30% (V/V) ratio with epoxychloropropane, 1,2-Ethylene glycol diglycidyl ether or 1, the 2-butanediol diglycidyl ether is dissolved in the tetrachloroethylene, obtain containing cross-linking agent epoxychloropropane, 1,2-Ethylene glycol diglycidyl ether or 1, the tetrachloroethylene solution of 2-butanediol diglycidyl ether;
2) be 1 with beta-schardinger dextrin-and tetrachloroethylene solution by the ratio of quality and volume: 1-20 (g/mL), the tetrachloroethylene solution that beta-schardinger dextrin-is added the step 1) preparation, solution mixes, be standard again with the beta-schardinger dextrin-, ratio in quality and volume is 1: the ratio of 0.1-5 (g/mL) slowly drips 37% concentrated hydrochloric acid, 98% concentrated nitric acid, 98% sulphuric acid or perchloric acid while stirring, bath temperature remains on 20-80 ℃, reacts 1-48h, obtains the bile acid adsorbent of beta cyclo dextrin polymer.
The invention has the advantages that: it is convenient to make raw material sources, and low price, preparation technology are simple, and prepared adsorbents adsorb speed is fast, binding ability strong, difficult drop-off, and has no side effect.
The specific embodiment
With embodiment the present invention is illustrated below.
Example 1
Take by weighing the 2g beta-schardinger dextrin-, add 10mL cross-linking agent Ethylene glycol diglycidyl ether, bath temperature remains on 90 ℃, slowly drips 98% concentrated sulphuric acid 1mL while stirring, and slow reaction 4h obtains the beta cyclo dextrin polymer adsorbent.
Example 2
Get the 3g beta-schardinger dextrin-, add 20mL cross-linking agent epoxychloropropane, bath temperature remains on 60 ℃, slowly drips 98% concentrated nitric acid 5mL while stirring, and slow reaction 2h obtains the beta cyclo dextrin polymer adsorbent.
Example 3
Get the 2g beta-schardinger dextrin-, add 40mL cross-linking agent 1,2-butanediol diglycidyl ether, bath temperature remain on 10 ℃, slowly drip 37% concentrated hydrochloric acid 10mL while stirring, and slow reaction 16h obtains the beta cyclo dextrin polymer adsorbent.
Example 4
Get the 3g beta-schardinger dextrin-, add 30mL cross-linking agent epoxychloropropane, bath temperature remains on 60 ℃, slowly drips perchloric acid 0.3mL while stirring, and slow reaction 16h obtains the beta cyclo dextrin polymer adsorbent.
Example 5
Take by weighing the 4g beta-schardinger dextrin-, add epoxychloropropane-tetrachloroethylene solution 20mL of 10%, slowly drip 37% concentrated hydrochloric acid 10mL while stirring, bath temperature remains on 80 ℃, and reaction 10h obtains the beta cyclo dextrin polymer adsorbent.
Example 6
Take by weighing the 4g beta-schardinger dextrin-, add Ethylene glycol diglycidyl ether-tetrachloroethylene solution 20mL of 20%, slowly drip 98% concentrated sulphuric acid 20mL while stirring, bath temperature remains on 40 ℃, and reaction 4h obtains the beta cyclo dextrin polymer adsorbent.
Example 7
Take by weighing the 4g beta-schardinger dextrin-, 1 of adding 30%, 2-butanediol diglycidyl ether-tetrachloroethylene solution 80mL slowly drips 98% concentrated nitric acid 15mL while stirring, and bath temperature remains on 60 ℃, and reaction 24h obtains the beta cyclo dextrin polymer adsorbent.
Example 8
Take by weighing the 4g beta-schardinger dextrin-, add 30% Ethylene glycol diglycidyl ether-tetrachloroethylene solution 20mL, slowly drip perchloric acid 7mL while stirring, bath temperature remains on 20 ℃, and reaction 48h obtains the beta cyclo dextrin polymer adsorbent.
Claims (2)
1. the preparation method of the bile acid adsorbent of a beta cyclo dextrin polymer, its feature comprises following process:
With beta-schardinger dextrin-and cross-linking agent epoxychloropropane, 1,2-Ethylene glycol diglycidyl ether or 1, the 2-butanediol diglycidyl ether is 1 according to the ratio of quality gram and volume milliliter: the ratio of 1-20, with beta-schardinger dextrin-and cross-linking agent epoxychloropropane, 1,2-Ethylene glycol diglycidyl ether or 1, the 2-butanediol diglycidyl ether mixes; Be standard again with the beta-schardinger dextrin-, ratio in quality gram and volume milliliter is 1: the ratio of 0.1-5 slowly drips 37% concentrated hydrochloric acid, 98% concentrated nitric acid, 98% sulphuric acid or perchloric acid while stirring, slowly stir 10-90 ℃ of reaction 1-20h, obtain the bile acid adsorbent of beta cyclo dextrin polymer.
2. the preparation method of the bile acid adsorbent of a beta cyclo dextrin polymer, its feature comprises following process:
1) be that 1-30% is with epoxychloropropane, 1 according to volume ratio earlier, 2-Ethylene glycol diglycidyl ether or 1, the 2-butanediol diglycidyl ether is dissolved in the tetrachloroethylene, obtain containing cross-linking agent epoxychloropropane, 1,2-Ethylene glycol diglycidyl ether or 1, the tetrachloroethylene solution of 2-butanediol diglycidyl ether;
2) the tetrachloroethylene solution that beta-schardinger dextrin-and step 1) are made is 1 in the ratio of quality gram and volume milliliter: the ratio of 1-20, beta-schardinger dextrin-is added tetrachloroethylene solution, solution mixes, be standard again with the beta-schardinger dextrin-, ratio in quality gram and volume milliliter is 1: the ratio of 0.1-5 slowly drips 37% concentrated hydrochloric acid, 98% concentrated nitric acid, 98% sulphuric acid or perchloric acid while stirring, bath temperature remains on 20-80 ℃, reacts 1-24h, obtains the bile acid adsorbent of beta cyclo dextrin polymer.
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| CNB200610013725XA CN100384479C (en) | 2006-05-17 | 2006-05-17 | Method for preparing bile acid adsorbent of beta cyclo dextrin polymer |
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| CNB200610013725XA CN100384479C (en) | 2006-05-17 | 2006-05-17 | Method for preparing bile acid adsorbent of beta cyclo dextrin polymer |
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| CN100384479C true CN100384479C (en) | 2008-04-30 |
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Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104140544A (en) * | 2013-05-10 | 2014-11-12 | 国家纳米科学中心 | Cyclodextrin porous nanocapsule, and preparation method and use thereof |
| CN115124729B (en) * | 2022-07-18 | 2023-03-21 | 华南理工大学 | Cross-linking agent based on beta-cyclodextrin and bile acid and preparation method and application thereof |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10195108A (en) * | 1997-01-09 | 1998-07-28 | Makoto Komiyama | Method for synthesizing crosslinked cyclodextrin polymer and removal of cholesterol with the polymer |
| JP2003226737A (en) * | 2002-02-04 | 2003-08-12 | Maeda Seikan Kk | Cross-linked cyclodextrin and endocrine disrupter remover using the same |
| CN1541761A (en) * | 2003-04-30 | 2004-11-03 | 中国科学院大连化学物理研究所 | Cyclodextrin cross-linking polymeric microsphere capable of absorbing bilirubin and its preparation and application |
| CN1660129A (en) * | 2004-12-13 | 2005-08-31 | 天津大学 | Method for preparing agent of cyclodextrin-cellulose for adsorbing uric acid |
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- 2006-05-17 CN CNB200610013725XA patent/CN100384479C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH10195108A (en) * | 1997-01-09 | 1998-07-28 | Makoto Komiyama | Method for synthesizing crosslinked cyclodextrin polymer and removal of cholesterol with the polymer |
| JP2003226737A (en) * | 2002-02-04 | 2003-08-12 | Maeda Seikan Kk | Cross-linked cyclodextrin and endocrine disrupter remover using the same |
| CN1541761A (en) * | 2003-04-30 | 2004-11-03 | 中国科学院大连化学物理研究所 | Cyclodextrin cross-linking polymeric microsphere capable of absorbing bilirubin and its preparation and application |
| CN1660129A (en) * | 2004-12-13 | 2005-08-31 | 天津大学 | Method for preparing agent of cyclodextrin-cellulose for adsorbing uric acid |
Non-Patent Citations (4)
| Title |
|---|
| B-环糊精交联聚合物的合成及表征. 金文英等.桂林工学院学报，第25卷第3期. 2005 |
| B-环糊精交联聚合物的合成及表征. 金文英等.桂林工学院学报，第25卷第3期. 2005 * |
| B-环糊精聚合物与药物包合作用的研究. 吴文娟等.西北药学杂志，第17卷第2期. 2002 |
| B-环糊精聚合物与药物包合作用的研究. 吴文娟等.西北药学杂志，第17卷第2期. 2002 * |
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