CN101407532B - Method for preparing gardenin from gardenia - Google Patents
Method for preparing gardenin from gardenia Download PDFInfo
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- CN101407532B CN101407532B CN2008101624030A CN200810162403A CN101407532B CN 101407532 B CN101407532 B CN 101407532B CN 2008101624030 A CN2008101624030 A CN 2008101624030A CN 200810162403 A CN200810162403 A CN 200810162403A CN 101407532 B CN101407532 B CN 101407532B
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- soup
- jasminoidin
- ethanol
- cape jasmine
- gardenia
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/582—Recycling of unreacted starting or intermediate materials
Abstract
The invention discloses a method for using gardenia as the material for preparing gardenoside, which uses different strong-weak abilities of adsorbing other components and gardenoside in gardenia extract by HPD-100 type microporous resin for loading samples by a certain speed; and after being washed by an ethanol solution of different concentration and different eluting speeds, all the remain eluted medicine liquid is combined, and the gardenoside finished product can be prepared by spray drying. The extracted gardenia herb residue can be used as feed additives or fertilizers. The whole related technique does not produce solid waste residue and technique waste water, and is an environmental protection technique that is suitable for enterprise production applications. The method of using the gardenia as the material for preparing the gardenoside is good in product quality and high in economic value.
Description
Technical field
The present invention relates to a kind of preparation method of therefrom medicinal material extract effective constituent, especially, relating to a kind of is the method for feedstock production jasminoidin with cape jasmine.
Background technology
Cape jasmine, head is stated from＜Shennong Bencaojing〉name will pellet.Classify middle product＜Mingyi Bielu as〉be called and get over the peach,＜property of medicine opinion beginning title SHANZHIZI, mountain Cape jasmine, Gardenia claimed again.＜Tang materia medica〉claim branch again.Use and existing more than the 1600 year history of clinical treatment in China, existing with Rubiaceae evergreen shrubs plant cape jasmine＜GardeniaJasminotdes〉mature fruit be used as medicine, its bitter, cold in nature.The thoughts of returning home, liver, stomach through,, have clearing away heat and promoting diuresis, water pouring relieving restlessness, effects such as removing pattogenic heat from the blood and toxic material from the body.Be usually used in the pyreticosis restlessness of asrhenia type and insomnia, jaundice, gonorrhoea is quenched one's thirst, hot eyes, pharyngalgia is spitted blood, and the bloody flux eqpidemic disease is sprained disease such as swell and ache.Hepatic cholagogic arranged, promote pancreatic secretion, step-down, prevent and treat atherosclerosis and antithrombotic formation, the effect of antipyretic-antalgic, antibiotic and anti-inflammatory and treatment soft tissue injury, become active and immunity has restraining effect to fine, soft fur to mutagenic compound, and do not have carcinogenic, teratogenesis, mutagenic toxicity.Neurotrophic factor (NCF) is one of most important bioactive molecules of nerve system of human body, and the compound jasminoidin has promoter action to it in the cape jasmine, and neural anoxic is shielded.
Domestic and international confessed Chinese medicine cape jasmine effective constituent is the iridoids material, the contained iridoids material of cape jasmine comprises jasminoidin, Gardenoside, cape jasmine thuja acid etc., what wherein activeconstituents was the highest is jasminoidin, and the significant composition of cape jasmine medicinal material is a jasminoidin in the Chinese Pharmacopoeia.Jasminoidin is that utilization high-tech production technique is extracted the refining product that forms from the dry mature fruit of madder wort cape jasmine.Jasminoidin is the iridoid glycoside compounds, and different name Geniposide, plain glucoside geniposides of plum all, jasminoidin are again to produce gardenia blue, cape jasmine is red, cape jasmine is purple intermediate and the effective monomer of crude drug product.Therefore, separation, purifying, crystallization and the assay of jasminoidin become gordian technique to the cape jasmine deep development.
Jasminoidin also has multiple pharmaceutical usage, have the report pharmacological action to show: jasminoidin has effects such as laxative, analgesia, cholagogic, anti-inflammatory, treatment soft tissue injury and inhibition gastric secretion and reduction pancreatic amylase, also be the material medicine that is used for the treatment of diseases such as cardiovascular and cerebrovascular, liver and gall and diabetes, also can generate the increasing crop yield agent.
Chinese patent [application number CN200510026143] is a kind of, and to prepare the method, [application number CN200510026142] of high-purity gardenoside-prepare method, [application number CN200510026144]-a kind of three patents such as method with preparing total iridoid glycoside with cape jasmine fruit of jasminoidin, genipin-1-β-D-gentiobiose glycosides with cape jasmine fruit with cape jasmine fruit roughly the same, all with washing cyclenes ether terpene substances with low-concentration ethanol again behind big water gaging and 10% alcohol flushing, this technological process is relatively loaded down with trivial details, the preparation cost height.
Chinese patent [application number CN200310111038.8] a kind of Fructus Gardeniae extract and preparation technology thereof and its application the invention discloses a kind of Fructus Gardeniae extract, and it is to be the extract that contains iridoid glycoside of feedstock production with the Chinese medicine cape jasmine.The jasminoidin weight percentage is about 30% only in the gained Fructus Gardeniae extract, and content is relatively low.
Chinese patent [application number CN200510017378.3] discloses a kind of method of the comprehensive utilization of cape jasmine, wherein relates to the extraction of multiple composition in the separation of jasminoidin and the cape jasmine, has made full use of the cape jasmine resource, but its refining jasminoidin.
Begin one's study from the sixties in 20th century utilization of cape jasmine effective constituent only possess the ability of producing a small amount of jasminoidin product so far, and the supply of jasminoidin is in very well sold and in short supply state in the international market always.Simultaneously at home along with the improving constantly of modern life level and quality of life, " natural product " gains great popularity, and people more and more pay attention to natural medicine, especially treatment by Chinese herbs.Therefore, should carry out the comprehensive utilizating research of Fructus Gardeniae extract energetically, strengthen the application and development dynamics of cape jasmine product at aspects such as medicine, food.In a word, exploring exploitation cape jasmine series product has a extensive future.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, providing a kind of is the method for feedstock production jasminoidin with cape jasmine.
The objective of the invention is to be achieved through the following technical solutions: a kind of is the method for feedstock production jasminoidin with cape jasmine, may further comprise the steps:
(1) the cape jasmine crude drug is through section or be ground into meal, and the volume percent that adds 8～10 times of volumes is that 60% aqueous ethanol extracts each 1.5～2 hours 2～3 times;
(2) liquid behind the united extraction, centrifuging, filtrate decompression concentrates and reclaims ethanol to relative density of medicine liquid is 1.05;
(3) after the soup after will concentrating is diluted to sample soup A440 and reaches 60 with deionized water, last HPD-100 type macroporous resin column, sample speed is at 5～6 times upper prop macroporous resin volume per hour in the control, and applied sample amount and upper prop macroporous resin volume ratio are 1: 1; Soup behind the collection upper prop, behind the deionized water of one times of upper prop macroporous resin of soup wash-out volume, with volume percent is that 25% aqueous ethanol is eluted to elutriant A238 less than 0.8, collects elutriant, is 70% aqueous ethanol wash-out elutriant then with volume percent;
(4) remain soup after merging all wash-outs, after concentrating under reduced pressure reclaims ethanol, spray-dried jasminoidin.
The present invention gets beneficial effect: whole technological process only makes water and ethanol for extracting solvent, production process does not have waste water, waste gas to produce, used HPD-100 type macroporous resin and ethanol reagent are all recyclable to be utilized again, be fit to suitability for industrialized production, be a kind of environment-friendly type new technology, obtain high-purity natural product jasminoidin
Embodiment
The present invention is the method for feedstock production jasminoidin with cape jasmine, may further comprise the steps:
One, the cape jasmine crude drug is through cutting into slices or being ground into meal, and the aqueous ethanol that adds 8～10 times of volumes (volume percent is 60%) extracts each 1.5～2 hours 2～3 times.
Two, liquid behind the united extraction, through centrifuging, it is 1.05 that filtrate is reclaimed ethanol to relative density of medicine liquid through concentrating under reduced pressure.
Three, after the soup after will concentrating is diluted to sample soup A440 and reaches about 60 with deionized water, last HPD-100 type macroporous resin column, sample speed is at 5～6 times upper prop macroporous resin volume per hour in the control, applied sample amount (with the concentrated medicament volumeter) and upper prop macroporous resin volume ratio be 1: 1 so that other compositions except that jasminoidin in the abundant adsorbing and extracting soup of macroporous resin, 60% left and right sides jasminoidin is not by resin absorption in the last sample soup.Soup behind the collection upper prop, the deionized water of one times of upper prop macroporous resin of first wash-out volume after last sample finishes is with the flushing jasminoidin.Elution speed can be regulated increase.After the deionized water wash-out is collected and is finished, utilize the relative size of HPD-100 macroporous resin adsorption jasminoidin and other effective constituent ability, aqueous ethanol wash-out with 25% is by the jasminoidin of macroporous resin adsorption, was that (elution process is observed the elutriant color to the wash-out terminal point constantly with elutriant A238 less than 0.8 o'clock, with control speed and judgement wash-out terminal point), the complete back of wash-out jasminoidin remains effective constituent with the aqueous ethanol wash-out of 70% concentration, and elution speed can be regulated increase.
Four, remain soup after merging all wash-outs at last, spray-dried respectively jasminoidin after concentrating under reduced pressure reclaims ethanol.
Embodiment 1: the selection of solvent
Respectively get 100g cape jasmine medicinal material and test, extraction conditions sees the following form, and the result is as follows:
| Cape jasmine medicinal material amount amount | Extraction time | The solvent title | The solvent consumption | Solid content % | OD |
| 100 | 2 | Water 1000 | 1000 | 30.10 | 7.97 |
| 100 | 2 | 30% ethanol | 1000 | 30.08 | 5.66 |
| 100 | 2 | 60% ethanol | 1000 | 25.70 | 3.88 |
| 100 | 2 | 95% ethanol | 1000 | 23.72 | 2.65 |
The comprehensive table of going up is considered factors such as extraction cost and solid content, and it is optimum concn that 60% aqueous ethanol extracts.
Embodiment 2: the selection of extraction time
Get three parts of 100g cape jasmine medicinal materials, the aqueous ethanol with 60% extracts, and extracts twice, compares extracting 1 hour, 2 hours, 3 hours.
| The medicinal material amount | Extraction time | Time (hr) | Solvent consumption (ml) | Solid content % | OD |
| 100 | 2 | 1 | 60% ethanol 1000 | 25.70％ | 3.30 |
| 100 | 2 | 2 | 60% ethanol 1000 | 28.12％ | 3.41 |
| 100 | 2 | 3 | 60% ethanol 1000 | 28.5％ | 3.50 |
More than experiment shows: the aqueous ethanol with 60% extracts, and extracts twice, extracts 2 hours, basically can extracts active ingredients in the cape jasmine is complete, and extracting 3 hours yield does not have big variation basically.Embodiment 3: the selection of extraction time
Get three parts of 100g cape jasmine medicinal materials, the aqueous ethanol with 60% extracts, and each extraction time is 2 hours, compares extracting 1 time, 2 times, 3 times, and the result is as follows:
| The medicinal material amount | Extraction time | Time (hr) | Solvent consumption (ml) | Solid content % | OD |
| 100 | 1 | 2 | 60% ethanol 1000 | 20.50％ | 3.30 |
| 100 | 2 | 2 | 60% ethanol 1000 | 28.12％ | 3.41 |
| 100 | 3 | 2 | 60% ethanol 1000 | 28.7％ | 3.55 |
As can be seen from the above table, extract most of mast extracts active ingredients that just can make for twice in the mast fruit and come out, but comprehensively gain and loss is according to practical situation, it is secondary to three that the present invention adopts extraction time.
Embodiment 4: the experimental study of soup centrifugal test
Soup can obviously be removed the visible floss impurity of a large amount of naked eyes after centrifugal
Embodiment 5: the selection experimental study of resin model
Select the macroporous resin of HPD-100, HPD-80, HPD-400, D-101, X-5 model to compare according to the character of Gardenia Yellow and jasminoidin
Respectively get 10g and add in the 100ml beaker, add (A238=178.3, A440=50.9, OD=3.5) 80ml in the soup, static absorption through pretreated resin.Detect the soup parameter after 3 hours.The results are shown in following table:
| HPD-80 | HPD-100 | HPD-400 | D-101 | X-5 | |
| A238 | 53.1 | 70.0 | 74.7 | 89.1 | 45.2 |
| A440 | 16.4 | 18.0 | 19.8 | 21.0 | 14.7 |
| OD | 3.24 | 3.88 | 3.77 | 4.24 | 3.07 |
Analyze: X-5 is stronger to jasminoidin and other effective constituent adsorptive power, and selectivity is not high, is unfavorable for water flushing in early stage jasminoidin.Therefore comprehensively relatively select HPD-100 to do subsequent experimental.
Embodiment 6: the selection experimental study of going up sample cape jasmine soup diluting solvent
Adopt the different solvents dilute liquid medicine, get the soup that the 10g resin is soaked in same amount, carry out standing adsorption relatively, the results are shown in following table
| Water | 25% ethanol | 30% ethanol | 40% ethanol | |
| A440 before the absorption | 50.9 | 49.0 | 47.6 | 46.8 |
| A440 behind the absorption 3h | 12.4 | 20.6 | 29.5 | 23.0 |
The macroporous resin adsorption ability exists saturated, and other composition is big more by the amount of macroporous resin adsorption in the soup, and the amount of then representing jasminoidin to be adsorbed is more little, and just favourable more and water elution jasminoidin in early stage are so directly the dilute with water upper prop both can.
Embodiment 7: the selection experimental study of sample solution concentration:
The absorption of resin is a process of selecting absorption, and too high concentration must influence absorption, and concentration is crossed the low adsorption time prolongation that will inevitably make, thereby lowers efficiency.This experiment is by flow going up the method for sample, uses the soup upper prop (20ml resin pack into 30*1.6cm post) of different concns.By detecting, be last sample terminal point with effluent liquid A440=2.Investigating the absorption of A440 in the 40-80 concentration range changes.
| Sample solution concentration A440 | 40 | 50 | 60 | 70 | 80 |
| Last sample volume ml | 395 | 300 | 235 | 185 | 135 |
| Total applied sample amount | 15800 | 15000 | 14100 | 12950 | 10800 |
Annotate; Total applied sample amount is gone up the sample volumeter with A440*
Last table analysis can get, and sample solution concentration A440 should be chosen between the 50-70.In conjunction with the comprehensive gain and loss of every experiment, upper prop when selecting soup to be diluted to A440=60, other effective constituent adsorptive capacitys are relatively large in the soup, favourable and water elution jasminoidin in early stage.
Embodiment 8: the selection experimental study of elutriant
With A440 is 60 aqueous solution upper prop (20ml resin pack into 30*1.6cm post), calculates total applied sample amount.Respectively with 500ml Different concentrations of alcohol wash-out.Calculate the content of each elutriant.
Sample 250ml dilution back soup on each, water and the test of different concentration ethanol elutriant massive parallel the results are shown in following table:
| Water | 10％ | 20％ | 25％ | 30％ | 35％ | 70％ | 90％ | 100％ | |
| Pigment content (mg) | --－ | --- | --- | 20.7 | 31.1 | 102.4 | 343.7 | 392.1 | 401.6 |
| 0D | 72.54.1 | 310-517 | 582.3-73 | 677-53.4 | 483.7-57.4 | 209.4-0.7 | 2.1 | 2.3 | 2.1 |
Greater than other effective constituent, 35% ethanol is relatively poor to both selectivity to the selectivity of jasminoidin for water, 10%, 20%, 25%, 30% ethanol, and 70%, 90%, 100% ethanol is to both non-selectivities almost.Therefore selection is taken off jasminoidin with massive laundering earlier, then remains effective constituent with 70% ethanol elution of high density more afterwards with 25% ethanol elution jasminoidin, thereby reaches the purpose of refining jasminoidin.
Embodiment 9:
The bright medicinal material of 10KG cape jasmine gets soup 3140ml after 60% ethanol (by volume) extraction concentrates, get 1750ml soup (containing jasminoidin 93537.5mg) and be diluted to upward 1500mlHPD-100 macroporous resin of A440=60 with deionized water, (the about 60000ml of the medicine liquid volume that loses shape, contain jasminoidin 58464mg behind the upper prop in the soup, account for soup jasminoidin total content 62.5%), after last sample finishes, earlier with deionized water wash-out resin absorption water-soluble impurity, (elutriant contains jasminoidin 22478.38mg to the jasminoidin of using (water lotion contains jasminoidin 4209.75mg) 25% ethanol (by volume) flushing resin absorption again less than 0.8 to elutriant A238, account for 24% of total content in the soup, so far about jasminoidin of about 91% separates from soup), follow ethanol elution residue effective constituent with 70%, remain soup after merging all wash-outs, after spray-dried about 44.8g jasminoidin and other effective constituents of the 100g left and right sides.
Claims (1)
1. one kind is the method for feedstock production jasminoidin with cape jasmine, it is characterized in that, may further comprise the steps:
(1) the cape jasmine crude drug is through cutting into slices or being ground into meal, and the aqueous ethanol that adds 8～10 times of volumes extracts each 1.5～2 hours 2～3 times; The alcoholic acid volume percent is 60% in the described aqueous ethanol;
(2) liquid behind the united extraction, centrifuging, filtrate decompression concentrates and reclaims ethanol to relative density of medicine liquid is 1.05;
(3) after the soup after will concentrating is diluted to sample soup A440 and reaches 60 with deionized water, last HPD-100 type macroporous resin column, sample speed is at 5～6 times upper prop macroporous resin volume per hour in the control, and applied sample amount and upper prop macroporous resin volume ratio are 1: 1; Soup behind the collection upper prop, behind the deionized water of one times of upper prop macroporous resin of soup wash-out volume, with volume percent is that 25% aqueous ethanol is eluted to elutriant A238 less than 0.8, collects elutriant, is that 70% aqueous ethanol wash-out remains effective constituent with volume percent then;
(4) remain soup after merging all wash-outs, after concentrating under reduced pressure reclaims ethanol, spray-dried jasminoidin.
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Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103372078A (en) * | 2012-04-19 | 2013-10-30 | 中国中医科学院中药研究所 | Medicine for treating influenza and preparation method thereof |
| CN108929350A (en) * | 2018-05-25 | 2018-12-04 | 无锡济民可信山禾药业股份有限公司 | A method of it distills to extract from XINGNAOJING ZHUSHEYE and recycles Gardenoside in waste liquid |
| CN110090251B (en) * | 2019-06-03 | 2021-07-06 | 扬子江药业集团上海海尼药业有限公司 | Preparation method of artemisia capillaris tablet |
| CN111617127A (en) * | 2020-06-24 | 2020-09-04 | 鲁南制药集团股份有限公司 | A pharmaceutical composition for treating icterohepatitis with syndrome of dampness-heat in liver and gallbladder, and its preparation method |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1706859A (en) * | 2005-05-24 | 2005-12-14 | 中国人民解放军第二军医大学 | Process of preparing high-purity jasminodin with Cape jasmine fruit |
| CN1807441A (en) * | 2006-02-23 | 2006-07-26 | 江南大学 | Method for producing high purity jasminoidin and high color number gardenia yellow pigment |
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- 2008-11-24 CN CN2008101624030A patent/CN101407532B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1706859A (en) * | 2005-05-24 | 2005-12-14 | 中国人民解放军第二军医大学 | Process of preparing high-purity jasminodin with Cape jasmine fruit |
| CN1807441A (en) * | 2006-02-23 | 2006-07-26 | 江南大学 | Method for producing high purity jasminoidin and high color number gardenia yellow pigment |
Non-Patent Citations (3)
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| 涂盛辉等.从栀子黄废液中分离富集栀子苷的研究.《中成药》.2008,第30卷(第1期),56-60. * |
| 涂盛辉等.大孔吸附树脂精制中药栀子中栀子苷的研究.《南昌大学学报 工科版》.2007,第29卷(第4期),307-310. * |
| 董磊等.大孔吸附树脂对栀子苷精制纯化的研究.《河南大学学报（医学版）》.2006,第25卷(第4期),27-29. * |
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