CN102764282A - Method for extracting and separating tannins components of immature fruits of medicine terminalia - Google Patents
Method for extracting and separating tannins components of immature fruits of medicine terminalia Download PDFInfo
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- CN102764282A CN102764282A CN2012102843455A CN201210284345A CN102764282A CN 102764282 A CN102764282 A CN 102764282A CN 2012102843455 A CN2012102843455 A CN 2012102843455A CN 201210284345 A CN201210284345 A CN 201210284345A CN 102764282 A CN102764282 A CN 102764282A
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- ethyl acetate
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- immature fruits
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Abstract
The invention discloses a method for extracting and separating tannins components of immature fruits of medicine terminalia. The method includes the steps of firstly, taking medicinal materials of the immature fruits of the medicine terminalia, crushing the medicinal materials, using an acetone solution as an extracting agent, adding the acetone solution with the volume 2-6 times of the volume of the medicinal materials, performing extraction for 2-4 times by using a room temperature immersion method, combining extract liquids and concentrating the extract liquids into extractum; secondly, extracting the extractum by using a small amount of ethyl acetate for a plurality of times, combining ethyl acetate extract liquids, and concentrating the ethyl acetate extract liquids until the extract liquids are free of ethyl acetate odors; and thirdly, using methyl alcohol to redissolve concentrated substances, adding a macroreticular resin column, using a methyl alcohol aqueous solution for eluting the substances and concentrating and drying eluent to obtain tannins extractives of the immature fruits of the medicine terminalia. The tannins component content of the extractives is larger than 80%, a method for determining tannin contents refers to a phosphomolybdium tungstic acid-casein method for determining the tannin contents, and the phosphomolybdium tungstic acid-casein method is recorded in the first part addendum XB of Chinese pharmacopoeia 2010 edition. The method for extracting and separating the tannins components of the immature fruits of medicine terminalia is small in solvent consumption, high in efficiency, high in content and applicable to industrial mass production.
Description
Technical field
The present invention relates to a kind of extraction, purification process of Chinese medicinal components, specifically, be meant that FRUCTUS TERMINALIAE IMMATURUS (also claiming Fructus chebulae immaturus, Tibet Fructus Canarii) extracts, purification tannin constituents.
Background technology
Chinese Pharmacopoeia records the dry young fruit that the medical material FRUCTUS TERMINALIAE IMMATURUS derives from Combretum Racemosum plant Fructus Chebulae Terminalia chebula Retz..Its property is bitter, sour, puckery, flat, returns lung, large intestine channel.Have clearing away heat and promoting production of body fluid, the antidotal effect is mainly used in the treatment of pneumonia, laryngitis, tonsillitis and bacillary dysentery and acute enteritis etc. clinically.Its main chemical compositions is tannin phenolic acids, triterpenes and volatile oil etc., and wherein the content of tannin constituents and its pharmacologically active are closely related, are one of its important active component.So the tannin constituents in the extraction FRUCTUS TERMINALIAE IMMATURUS is used to develop produce markets such as medicine, sterilized articles therefrom, health food and has a high potential.
CN200510042885.2 discloses method for preparing and the application that the effective site of extracting in the FRUCTUS TERMINALIAE IMMATURUS is used for antibacterial and disease of viral infection; Three kinds of method for preparinies of main employing have been extracted the phenolic acid compound in the FRUCTUS TERMINALIAE IMMATURUS and have been used for antibacterial and viral infection; But wherein decocting method and circumfluence method all adopt the mode of heating, make the tannin constituents heating and decomposition in the FRUCTUS TERMINALIAE IMMATURUS easily; And another percolation consumes big, the time-consuming length of quantity of solvent, operation is cumbersome.Extract the tannin constituents in the FRUCTUS TERMINALIAE IMMATURUS so the invention discloses a kind of room temperature direct impregnation extraction method, dry through concentrating under reduced pressure, guaranteed the relatively stable of tannin constituents.Technological solvent-oil ratio disclosed by the invention is less, the content of tannin height of carrying, and efficient is high, energy savings, cheap, resin can reuse, and is easy to industrialized great production.
Summary of the invention
The object of the present invention is to provide a kind of is raw material with the FRUCTUS TERMINALIAE IMMATURUS, the method for extraction and purification of tannin constituents content＞80% in the extract.
The present invention implements through following concrete technical scheme.
FRUCTUS TERMINALIAE IMMATURUS tannin of the present invention is extracted, the method for purification, comprises the steps: in order
(1) get the FRUCTUS TERMINALIAE IMMATURUS medical material, pulverize, press the medical material volume and add 2-6 aqueous acetone solution doubly as extractant, the room temperature infusion process is extracted 2-4 time, merges lixiviating solution, simmer down to extractum;
(2) extractum is used a certain amount of ethyl acetate extraction, on a small quantity repeatedly, the combined ethyl acetate extracting solution is concentrated into no ethyl acetate abnormal smells from the patient;
(3) condensed matter is redissolved with methanol, last macroporous adsorptive resins is used the methanol aqueous solution eluting, and eluent concentrates, and drying promptly gets FRUCTUS TERMINALIAE IMMATURUS tannin extract.
Wherein the said aqueous acetone solution of step (1) refers to that percent by volume is concentration 60%-90%; The lixiviate duration is 24h-48h.
The described macroporous adsorbent resin of step (3) is main with the synthetic adsorbent resin of polystyrene mainly, comprises DiaionHP-20, SEPABEDS-SP825, SP850, SP700, SP70, SP207 etc.The said methanol aqueous solution concentration of volume percent of step (3) is 20%-80%.
With tannin constituents content＞80% that the inventive method is extracted, purification obtains, content of tannin is measured with reference to " content of tannin method for measuring among 2010 editions first appendix XB of Chinese pharmacopoeia adopts P-Mo-Wo acid-casein method to measure.Prepared FRUCTUS TERMINALIAE IMMATURUS tannin can separately or be share with other active component; With the various dosage forms that adjuvant such as starch, dextrin, lactose, microcrystalline Cellulose, hydroxypropyl methylcellulose, Polyethylene Glycol, magnesium stearate, differential silica gel, xylitol, glucose, glycine, mannitol, HP-etc. on any or more than one pharmaceuticss are mixed and made into, for example can process injection, tablet, slow releasing tablet, drop pill, granule, injectable powder, capsule.Preferred dosage form is chewable tablet, injectable powder, capsule.
Compared with prior art, technological solvent-oil ratio disclosed by the invention is less, the content of tannin height of carrying, and efficient is high, energy savings, cheap, resin can reuse, and is easy to industrialized great production.
The specific embodiment
In order to make the object of the invention, technical scheme and advantage clearer, will carry out detailed description to the preferred embodiments of the present invention below, but not be in order to limit scope of the present invention.
Embodiment one
Get FRUCTUS TERMINALIAE IMMATURUS medical material 450g, pulverize, add aqueous acetone solution, the room temperature dipping extracts three times continuously, adds 75% (v: the about 1.25L lixiviate of acetone soln v) 48 hours of 5 times of volumes for the first time; For the second time with added each lixiviate of acetone soln 1L of 80% for the third time respectively 24 hours, merge the lixiviate medicinal liquid, filter, filtrating in 45 ℃ of concentrating under reduced pressure is extractum.Use ethyl acetate extraction subsequently, add the 300ml ethyl acetate at every turn, extract the combined ethyl acetate extract 5 times; 40 ℃ of concentrating under reduced pressure are concentrated into no ethyl acetate abnormal smells from the patient, and condensed matter is redissolved with an amount of methanol (about 50ml) fully; Last Diaion HP-20 macroporous adsorbent resin (activation of resin elder generation) is used 20%, 40% and 60% (v: methanol aqueous solution eluting v), the methanol aqueous solution eluent of collection 60% successively; Obtain refined solution, 40 ℃ of concentrating under reduced pressure are with being placed in the constant temperature drying under reduced pressure case; Drying under reduced pressure promptly gets FRUCTUS TERMINALIAE IMMATURUS tannin extract 150g, content of tannin 92.5%.
Embodiment two
Get FRUCTUS TERMINALIAE IMMATURUS medical material 500g, be ground into fine powder, the aqueous acetone solution 1L of continuous three addings 85%, each lixiviate 24 hours merges lixiviating solution, filters, and filtrating in 40 ℃ of concentrating under reduced pressure is extractum.Use ethyl acetate extraction subsequently, each 250ml extracts the combined ethyl acetate extract 5 times; 40 ℃ are evaporated to no ethyl acetate abnormal smells from the patient, concentrate are redissolved last SEPABEDS-SP825 macroporous adsorbent resin (activation of resin elder generation) with methanol 100ml; Use 30%, 50%, 70% (v successively; Methanol aqueous solution eluting is v) collected 50% methanol aqueous solution eluent, obtains refined solution, 40 ℃ of concentrating under reduced pressure, and with being placed in the constant temperature drying under reduced pressure case, drying under reduced pressure gets FRUCTUS TERMINALIAE IMMATURUS tannin extract 200g, content of tannin 89.6%.
Embodiment three: the capsule for preparing the FRUCTUS TERMINALIAE IMMATURUS tannin by technical method well known in the art
Getting the FRUCTUS TERMINALIAE IMMATURUS tannin extract 100g of embodiment one, is filler with starch and dextrin, granulates as binding agent with 3% starch slurry, adds an amount of magnesium stearate, filled capsules, and every capsules contains FRUCTUS TERMINALIAE IMMATURUS tannin 100mg, and packing promptly gets.
Embodiment four: the chewable tablet for preparing the FRUCTUS TERMINALIAE IMMATURUS tannin by technical method well known in the art
Get the FRUCTUS TERMINALIAE IMMATURUS tannin extract 150g of embodiment two, add an amount of starch, sucrose, dextrin, Herba Menthae essence, mannitol mix homogeneously, the system granule adds the magnesium stearate mix homogeneously, tabletting, and every contains FRUCTUS TERMINALIAE IMMATURUS tannin 100mg, and packing promptly gets.
Should be understood that, concerning those of ordinary skills, can improve or conversion, and all these improvement and conversion all should belong to the protection domain of accompanying claims of the present invention according to above-mentioned explanation.
Claims (4)
1. the tannin constituents of FRUCTUS TERMINALIAE IMMATURUS extraction, separation method is characterized in that, may further comprise the steps:
(1) get the FRUCTUS TERMINALIAE IMMATURUS medical material, pulverize, press the medical material volume and add 2-6 aqueous acetone solution doubly as extractant, the room temperature infusion process is extracted 2-4 time, merges lixiviating solution, simmer down to extractum;
(2) extractum is used a certain amount of ethyl acetate extraction, on a small quantity repeatedly, the combined ethyl acetate extracting solution is concentrated into no ethyl acetate abnormal smells from the patient;
(3) condensed matter is redissolved with methanol, last macroporous adsorptive resins is used the methanol aqueous solution eluting, and eluent concentrates, and drying promptly gets FRUCTUS TERMINALIAE IMMATURUS tannin extract.
2. method according to claim 1 is characterized in that, in the said step (1), said aqueous acetone solution refers to that concentration of volume percent is 60%-90%; The lixiviate duration is 24h-48h.
3. method according to claim 1 is characterized in that, the described macroporous adsorbent resin of said step (3) is main with the synthetic adsorbent resin of polystyrene mainly.
4. method according to claim 1 is characterized in that, the said methanol aqueous solution concentration of volume percent of said step (3) is 20%-80%.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106509281A (en) * | 2016-12-21 | 2017-03-22 | 神农架林区中医医院 | campylandra chinensis sore-throat relieving tea and preparation method thereof |
| CN106619779A (en) * | 2017-02-17 | 2017-05-10 | 西南民族大学 | Lonicera rupicola tannin extraction method |
| CN109806205A (en) * | 2019-01-07 | 2019-05-28 | 惠州绵俪生物科技有限公司 | A kind of FRUCTUS TERMINALIAE IMMATURUS extract and its antibacterial application |
| CN114558042A (en) * | 2021-12-09 | 2022-05-31 | 澳门科技大学 | Extract of Terminalia chebula Retz and application thereof |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1723965A (en) * | 2005-07-01 | 2006-01-25 | 西安惠大医药有限公司 | Method and use for preparing medicine extracted myrobalan for treating diseases infected by bacteria or virus |
-
2012
- 2012-08-06 CN CN2012102843455A patent/CN102764282A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1723965A (en) * | 2005-07-01 | 2006-01-25 | 西安惠大医药有限公司 | Method and use for preparing medicine extracted myrobalan for treating diseases infected by bacteria or virus |
Non-Patent Citations (3)
| Title |
|---|
| 张燕等: "油菜籽饼中单宁的提取、分离与纯化制备", 《华中农业大学学报》, vol. 17, no. 3, 30 June 1998 (1998-06-30), pages 294 - 299 * |
| 王红等: "单宁的提取纯化技术研究进展", 《辽宁化工》, vol. 40, no. 8, 31 August 2011 (2011-08-31), pages 864 - 866 * |
| 颜玉贞等: "西青果药材及提取物液相指纹图谱的应用研究", 《中成药》, vol. 26, no. 8, 31 August 2004 (2004-08-31), pages 603 - 607 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106509281A (en) * | 2016-12-21 | 2017-03-22 | 神农架林区中医医院 | campylandra chinensis sore-throat relieving tea and preparation method thereof |
| CN106619779A (en) * | 2017-02-17 | 2017-05-10 | 西南民族大学 | Lonicera rupicola tannin extraction method |
| CN109806205A (en) * | 2019-01-07 | 2019-05-28 | 惠州绵俪生物科技有限公司 | A kind of FRUCTUS TERMINALIAE IMMATURUS extract and its antibacterial application |
| CN109806205B (en) * | 2019-01-07 | 2022-07-01 | 惠州绵俪生物科技有限公司 | Fructus chebulae immaturus extract and antibacterial application thereof |
| CN114558042A (en) * | 2021-12-09 | 2022-05-31 | 澳门科技大学 | Extract of Terminalia chebula Retz and application thereof |
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Application publication date: 20121107 |