CN1670037A - Complex utilization of Gardenia - Google Patents
Complex utilization of Gardenia Download PDFInfo
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- CN1670037A CN1670037A CNA2005100173783A CN200510017378A CN1670037A CN 1670037 A CN1670037 A CN 1670037A CN A2005100173783 A CNA2005100173783 A CN A2005100173783A CN 200510017378 A CN200510017378 A CN 200510017378A CN 1670037 A CN1670037 A CN 1670037A
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- ethanol
- cape jasmine
- chlorogenic acid
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- washing lotion
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A40/00—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production
- Y02A40/10—Adaptation technologies in agriculture, forestry, livestock or agroalimentary production in agriculture
- Y02A40/20—Fertilizers of biological origin, e.g. guano or fertilizers made from animal corpses
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- Medicines Containing Plant Substances (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a plants comprehensive utilization method, particularly relates to a method for extracting the effective component from a traditional medicine cape jasmine, which comprises: extracting using aqueous dilute ethanol from a cape jasmine, then through the several chemical industry arts combination containing microfiltering by the filtration and film technique, separating by faintly polar macroreticular adsorbent resins and faintly alkaline macroreticular adsorbent resins, to get the gardenia yellow, chlorogenic acid, genipside, gardenia raw polysaccharides, water-soluble amino acid and SDF, the residue also can be used as feed addictive or fertilizer. In the process, there is on solid waste and rare waste water.
Description
The present invention is a kind of new method combination, can be with this method with the pigment in the natural product cape jasmine, and iridoids, chlorogenic acid, polysaccharide substep in a raw material extracts, and residuum also can be made foodstuff additive and fertilizer.Waste water is seldom handled easily in process of production, and certain environment protection significance is arranged.Should belong to the natural product comprehensive utilization.
Cape jasmine is the dry mature fruit of madder tannin plant cape jasmine, and the present is a kind of crude drug commonly used.With regard to its chemical composition, can be divided into the four big classes that marketable value can be arranged: the one, pigment, representative are Gardenia Yellow; The 2nd, iridoids is as gardenoside, Geniposidic acid etc.; The 3rd, organic acid is as chlorogenic acid and ursolic acid; The 4th, polyose, water are carried Crude polysaccharides and are also contained protein and pectin.Last residuum also contains robust fibre, includes IDF (water insoluble dietary fiber), does not almost have what solid waste.Our patented method exactly with one group of component of these components from coming out, make full use of raw material and increase benefit to reach.And present method is used film and resin coupling, and waste liquid is also few, is a kind of environment-friendly type method.Be set forth in down respectively with regard to each class component now:
One, gardenin class: representative is crocetin and disaccharide (gentiobiose) glucoside thereof, also has the flavonoid of a small amount of colour developing.Structural formula such as right figure:
A surname's carthamin (Crocin, Crocin): C
44H
64O
24, M=977.00, soluble in water, be slightly soluble in organic solvent.
Zang Honghua acid
Two, iridoids: representative is jasminoidin and Geniposidic acid, structural formula such as right figure:
Jasminoidin (Geniposide): M=388.36, m.p.163～164 ℃ jasminoidin: R=CH
3C
17H
24O
10Geniposidic acid: R=H C
16H
22O
10M=374 34
Three, organic acid: the physiologically active composition of representative is a chlorogenic acid, also has a small amount of ursolic acid, chlorogenic acid textural property such as right figure:
M.p.208 ℃ of chlorogenic acid (Chlorogenic acid), M=354.30,25 ℃ of water solubilities 4%, the heating for dissolving degree strengthens, and is soluble in ethanol, acetone, is slightly soluble in ethyl acetate, and semihydrate is a needle crystal, 110 ℃ of dehydrations.
Chlorogenic acid also is a kind of medicine if separate separately; If can separate not goodly, be easy to sneak into and disturbed the pigment quality in the gardenin, therefore in outlet level high quality pigment product, strict its amount that limit.
Four, polyose: the cape jasmine polysaccharide also is a kind of immunocompetence thing, if use water extraction, has a large amount of protein, the pectin class together proposes, and needn't carefully separate also available as protective foods.
Bits after all the other extract also can some Mierocrystalline cellulose (including water insoluble dietary fiber), but few because of measuring, and from economic implications, extracts and has not had profit.But recrement as fertilizer sources or screening back are also still passable as animal feedstuff additive.
Method of the present invention is exactly the composition that above four classes is had economic worth, and substep puts forward from a cape jasmine raw material, only extracts Gardenia Yellow, CN1466951 than prior art such as CN1544532 and only extracts the iridoids progress again.We integrate it, use the ultra-filtration membrane isolation technique with reduction ethanol consumption, and chlorogenic acid, Crude polysaccharides are also separated comprehensive utilization, have obviously increased economic benefit, and waste residue has also provided purposes, does not just have solid waste, has certain environment protection significance.
A purpose of this patent is, a kind of working method to cape jasmine fruit is provided, and can obtain gardenin, gardenoside, chlorogenic acid and Crude polysaccharides simultaneously with this method in a cape jasmine, last residuum additive also capable of using as feed or fertilizer.
Second purpose of this patent be, extracting, the ultrafiltration membrane technique of comprehensive modern chemical industry, and the macroporous adsorbent resin isolation technique combines, so that more economically effectively obtain valuable composition in the cape jasmine, waste residue and waste water seldom occur, is beneficial to environmental protection.
The purpose of this patent reaches by following steps:
1, at first use 50 ± 10% aqueous ethanol to soak the cape jasmine fruit that has been broken into 3-5mm, solid-liquid ratio is 1: 6～12.Soaking and stirring 6～16 hours is placed as 1# with solution after the filtration.Use again with the concentration aqueous alcohol with solid-liquid ratio 1: 3～8 soaking and stirring 6～8 hours again as method.Solution after the filtration and 1# filtrate merge, and steam in thin-film evaporator to ethanol content＜8%, and cooling is for further processing then.
2, be that 2～80,000 ultra-filtration membrane carries out ultrafiltration with the above-mentioned alcoholic acid cape jasmine vat liquor that boils off by molecular weight cut-off, collect filtrate upper prop (column material low-pole macroporous adsorbent resin), the control flow velocity makes it abundant absorption, collecting absorption back liquid is A, then crossing post with distilled water gets washing lotion B, use 30 ± 10% ethanol to wash post at last, get washing lotion C.Elutriant A, the B, the C that cross post are merged, promptly get gardenoside and the thick liquid of chlorogenic acid after concentrating.To the resin column of washing, colourless to effluent liquid with 95% ethanol elution.Concentrate and boil off ethanol, be drying to obtain the Gardenia Yellow powder.Commodity selling can be done in its look valency＞100, and chlorogenic acid content is low.
3, gardenoside and the thick liquid of chlorogenic acid are filtered, last weakly alkaline macroporous resin column, this moment, column material was adsorbed in the resin greater than iridoid glycosides the chlorogenic acid adsorptive power.Clean the ethanol elution of back with pH≤7, control flow velocity and pH wash out glucoside earlier, boil off ethanol and promptly get the gardenoside that iridoids is the master, use the aqueous ethanol of pH＜3 to clean pillar again, get washing lotion, boil off the ethanol condensing crystal filter chlorogenic acid, surplus liquid concentrates, refrigerator is put coldly, crystallization goes out a little chlorogenic acids again.
4, polysaccharide extracts: with the remaining cape jasmine slag of step 1, add 10～15 times of water yields, boiled two hours, filtered while hot, concentrated filtrate is put 95% ethanol that cold back adds 3 times of volumes, at this moment translucent flocks.Filter, will precipitate vacuum-drying and promptly get Crude polysaccharides.
5, survey the OD value: the OD value is gardenoside 237nm and the Gardenia Yellow ratio at the maximum absorbance at 440nm place, and it has represented the purity of Gardenia Yellow.High-quality Gardenia Yellow has strict requirement to the OD value, and export standard at least should be below 0.4.Our this method can reach above-mentioned requirements.
The following embodiment that does by a laboratory further specifies it
Take by weighing water content and be 9.17% commercially available Chinese medicine cape jasmine 10.0 grams, be broken into the 5mm fritter, be placed in the 500ml beaker, add 50% ethanol 100ml lixiviate 8 hours (irregularly stirring) in leaching process, placement adds 40% ethanol lixiviate 6 hours after filtering again, be merged filtrate after the filtration, boil off ethanol, adding water to 100ml is 60,000 hollow fiber ultrafiltration membrane by molecular weight cut-off, and this moment, liquid was golden red, prepare upper prop, filter residue is carried polysaccharide fully.
On the band piston glass separator column of a φ 20 * 500, wet method is loaded onto new brand of D100 type low-pole macropore separation resin in the morning of handling, above-mentioned golden red is crossed film liquid upper prop, the control flow velocity is about 0.5ml/min, collect absorption back liquid A, then crossing post with 50ml distilled water gets washing lotion B, cross post with 30% ethanol 60ml at last and get washing lotion C, be merged A, B, three parts of liquid of C, be used for further separating gardenoside (iridoids) and chlorogenic acid, crossing post with 95% ethanol afterwards, to wash Gardenia Yellow colourless to elutant, boils off ethanol, and excess vacuum-drying promptly gets Gardenia Yellow.Recording its look valency according to standard method is 130.Can make commodity greater than 60, survey its OD value again and be 0.196 and be high-quality product far below 0.4, the estimation productive rate of weighing is 8.8%.
On the little glass separator column of another φ 18 * 250, load onto the board D310R of Nankai weakly alkaline macroporous adsorbent resin, carry out pre-treatment by producer's requirement, afterwards with about half volume of above-mentioned A, B, C mixed solution inspissation on rotatory evaporator, filter upper prop, crossing post with 0.8～1.0ml/min speed adsorbs, absorption back fully washes gardenoside with 75% ethanol of pH6～7 that contain small amount of acetic acid earlier, get gardenoside after boiling off the ethanol drying, colourity is shallow than commercially available product, transfers 15% ethanol pH to 1～2 with sulfuric acid or hydrochloric acid more afterwards.Upper prop washes chlorogenic acid, places after the inspissation, filter some thick chlorogenic acids, the mother liquor reconcentration is put into refrigerator, can get a little chlorogenic acid crystallizations again in second day, merges two parts of chlorogenic acids and weighs to such an extent that yield is 0.4%, the gardenoside yield is 2.6%.
With the cape jasmine slag after the alcohol extracting, add distilled water 200ml and in the 500ml beaker, boil also constantly stirring in two hours, filtered while hot, this moment filtrate about 120ml, put cold after, with the adding gradually under agitation of 360ml95% ethanol, have translucent floss to coagulate this moment, filter the back and dry in vacuum drying oven, darken, weighing and calculating the Crude polysaccharides yield is 4.6%.Also have amino acid in the residual solution, water-soluble dietary fibre etc., calculating dry-matter is 4.65%.If after the drying be a kind of valuable fodder additives.
Last remaining solid slag is Mierocrystalline cellulose, xylogen etc., can make fodder additives or fertilizer, and so far cape jasmine is applied whole the separation, has not had solid waste, and liquid waste water is also few in the production process.This technology value of environmental protection is quite high.
Reference
[1].Shinji?Soeda，Takashi?Ochiai，Hiroyuki?Tanaka.[J].Life?Science，2001，69(24)：2887～2898.
[2].Kazuho?Abe，Minoru?Sugiura.[J]Byain?Research，1998，787(1)：132～138.
[3]. Wang Chuan pah, meter is built bright, Wang Lianghua, NKA macroporous adsorbent resin separate Gardenia Yellow .[J]. chemical industry progress .2003.22 (6): 622～625.
[4]. upright flourish, Gong Jianfu, Zhang Renzhi, TLC and column chromatography separate the comparison .[J of gardenoside]. Chinese materia medica Leader, Hunan .1998.4 (10): 33～35.
[5]. Guo Kelin, Shi Zuoqing, HeBing Lin, the Separation ﹠ Purification .[J of Gardenia Yellow]. Food Additives Used in China .1996. (2): 4～7.
[6]. Cao Linqing, Shi Rongqiu, the extraction of Gardenia Yellow and performance study .[J]. Henan chemical industry .2002. (10): 19～20.
[7]. Xie Xuejian, Zhang Junhui, horse Aiwa, Chinese medicine cape jasmine progress [J]. hour hands traditional Chinese medical science traditional Chinese medicines .2000.11 (10): 943～944.
Claims (4)
1. cape jasmine comprehensive utilization method.Its feature is the particle that earlier cape jasmine fruit is broken into 3～5mm, the aqueous ethanol of adding 50 ± 10%, the control solid-liquid ratio is 1: 6～12, stir and soaked 6～16 hours, it is standby to filter the back, and then with the water alcohol of same concentration, control solid-liquid ratio 1: 3～8 stirs and soaked 6～8 hours, solution after the filtration and above-mentioned solution merge, steam ethanol and took out cooling to＜8% o'clock, be that 2～80,000 ultra-filtration membrane carries out ultrafiltration by molecular weight cut-off afterwards, collect filtrate and go up low-pole macroporous adsorptive resins fractionation by adsorption that filter residue is in order to carry Crude polysaccharides.
2. ultrafiltrated as claimed in claim 1 is handled, its feature is to use the low-pole macroporous resin column, filtrate is controlled the flow velocity upper prop fully adsorbs, must flow out elutriant A, then crossing post with distilled water gets washing lotion B, use 30 ± 10% ethanol elutions to get washing lotion C at last, elutriant A, the B, the C that cross post are merged, get gardenoside and the thick liquid of chlorogenic acid after concentrating, to the resin column of washing, it is colourless fully to be eluted to washing lotion with 95% ethanol, collects the filtrate concentrate drying and promptly gets the Gardenia Yellow powder, its look valency＞100, chlorogenic acid content is low.
3. as claimed in claim 2 the thick liquid of gardenoside and chlorogenic acid is separated, its feature is with weakly alkaline macroporous adsorbent resin dress post, and with above-mentioned thick liquid upper prop, fully after the absorption, elder generation goes out iridoid glycosides with the neutral alcohol wash-out; Use the acidic ethanol of pH＜3 to clean pillar again, with washing lotion steam ethanol concentrate chlorogenic acid.
4. as the cape jasmine slag behind the extraction using alcohol in the claim 1, carry Crude polysaccharides again, its feature is bits to be added 10～15 times of water yields boiled two hours, filtered while hot, concentrated filtrate is put 3 times of volumes of cold back adding 〉=95% ethanol, gets translucent flocks, filters final vacuum and is drying to obtain Crude polysaccharides, last bits can be done fodder additives or fertilizer, no solid waste.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2005100173783A CN1670037A (en) | 2005-02-24 | 2005-02-24 | Complex utilization of Gardenia |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2005100173783A CN1670037A (en) | 2005-02-24 | 2005-02-24 | Complex utilization of Gardenia |
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| CN1670037A true CN1670037A (en) | 2005-09-21 |
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939459B (en) * | 2006-09-30 | 2010-05-19 | 福州大学 | Preparation of gardenia jasminoides by membrane separation technology |
| CN1939458B (en) * | 2006-09-30 | 2010-05-19 | 福州大学 | Preparation of gardenia jasminoides by macroporous adsorbing resin |
| CN101530491B (en) * | 2008-01-22 | 2012-09-19 | 上海中药制药技术有限公司 | Method of preparing gardenia extract by applying membrane filtration technology |
| CN103992905A (en) * | 2014-05-13 | 2014-08-20 | 秦广雍 | Preparation method of gardenia golden wine containing rich crocin and jasminoidin |
| CN105670335A (en) * | 2015-12-31 | 2016-06-15 | 江门市林业科学研究所 | Method for two-pot two stage countercurrent dynamic extraction of gardenia yellow pigment |
| CN110903677A (en) * | 2019-12-13 | 2020-03-24 | 九江学院 | Method for simultaneously preparing gardenia yellow pigment and blue pigment |
| CN111675923A (en) * | 2020-06-24 | 2020-09-18 | 河南大农联生物工程有限公司 | Method for extracting gardenia pigment through steam explosion and application method of extracted pigment |
| CN112010994A (en) * | 2020-08-07 | 2020-12-01 | 苏州大学 | Preparation method of gardenia pectin |
| CN112724277A (en) * | 2019-10-14 | 2021-04-30 | 湖北工业大学 | Preparation method of gardenia pectin, gardenoside and crocin |
-
2005
- 2005-02-24 CN CNA2005100173783A patent/CN1670037A/en active Pending
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1939459B (en) * | 2006-09-30 | 2010-05-19 | 福州大学 | Preparation of gardenia jasminoides by membrane separation technology |
| CN1939458B (en) * | 2006-09-30 | 2010-05-19 | 福州大学 | Preparation of gardenia jasminoides by macroporous adsorbing resin |
| CN101530491B (en) * | 2008-01-22 | 2012-09-19 | 上海中药制药技术有限公司 | Method of preparing gardenia extract by applying membrane filtration technology |
| CN103992905A (en) * | 2014-05-13 | 2014-08-20 | 秦广雍 | Preparation method of gardenia golden wine containing rich crocin and jasminoidin |
| CN105670335A (en) * | 2015-12-31 | 2016-06-15 | 江门市林业科学研究所 | Method for two-pot two stage countercurrent dynamic extraction of gardenia yellow pigment |
| CN112724277A (en) * | 2019-10-14 | 2021-04-30 | 湖北工业大学 | Preparation method of gardenia pectin, gardenoside and crocin |
| CN112724277B (en) * | 2019-10-14 | 2022-05-03 | 湖北工业大学 | Preparation method of gardenia pectin, gardenoside and crocin |
| CN110903677A (en) * | 2019-12-13 | 2020-03-24 | 九江学院 | Method for simultaneously preparing gardenia yellow pigment and blue pigment |
| CN111675923A (en) * | 2020-06-24 | 2020-09-18 | 河南大农联生物工程有限公司 | Method for extracting gardenia pigment through steam explosion and application method of extracted pigment |
| CN112010994A (en) * | 2020-08-07 | 2020-12-01 | 苏州大学 | Preparation method of gardenia pectin |
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