CN104262452A - Method for preparing obakulactone from waste liquid of extracting berberine from phellodendron bark - Google Patents
Method for preparing obakulactone from waste liquid of extracting berberine from phellodendron bark Download PDFInfo
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- CN104262452A CN104262452A CN201410481959.1A CN201410481959A CN104262452A CN 104262452 A CN104262452 A CN 104262452A CN 201410481959 A CN201410481959 A CN 201410481959A CN 104262452 A CN104262452 A CN 104262452A
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- obakulactone
- berberine
- ethanol
- filtrate
- waste liquid
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07J—STEROIDS
- C07J73/00—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms
- C07J73/008—Steroids in which the cyclopenta[a]hydrophenanthrene skeleton has been modified by substitution of one or two carbon atoms by hetero atoms by two hetero atoms
Abstract
The invention discloses a method for preparing obakulactone from an ethanol waste liquid of separating berberine from phellodendron bark, which comprises the following steps: by using a filtrate which is obtained by separating a crude product berberine from a phellodendron bark ethanol extracting solution as a raw material, carrying out enzymolysis with composite enzymes to obtain a precipitate, carrying out reflux extraction with ethanol, filtering to obtain a filtrate, and concentrating the filtrate under reduced pressure to recover ethanol to obtain a concentrated solution; and enriching the concentrated solution by a macroporous adsorbent resin process, eluting to obtain an eluate, concentrating the eluate, crystallizing and drying to obtain the obakulactone product. The yield of the obtained obakulactone is up to 0.35% (relative to the phellodendron raw material) or so, and the content is up to 80% above. The method can comprehensively utilize the phellodendron resources, changes wastes into valuable substances, reduces the environmental pollution, has the advantages of simple separation technique, high recovery rate and high limonin content, does not use any toxic organic solvent, is environment-friendly and is suitable for industrial production.
Description
Technical field
The present invention relates to a kind of method that waste liquid after Berberis Amurensis Rupr extraction Berberine prepares obakulactone, especially relate to a kind of enzyme treatment technique and extract from Berberis Amurensis Rupr the method preparing obakulactone the waste liquid after Berberine in conjunction with macroporous adsorbent resin isolation technique.
Background technology
Obakulactone is also known as obacalactone, limonene, dictamnolactone, it is a kind of triterpenes bitter principle, be mainly derived from the skin of rutaceae golden cypress (Phellodendron amurense Rupr.), the skin etc. of shaggy-fruited dittany (Dictamnus alba L.).Be proved to be and there is expelling parasite, antiulcer agent, hypoglycemic activity, intestinal tube can also be made to relax, the physiological functions such as the mouse sleep time that shortening α glucochloral and urethane cause.Golden cypress is the traditional medicine in China's Chinese medicine, has heat-clearing and damp-drying drug, and purging intense heat is except steaming, and the effects such as detoxification sore treatment, are mainly used in damp-heat dysentery, jaundice, and under band, heat is drenched, beriberi, hectic fever due to yin labor heat, night sweat, seminal emission, sore swollen toxin, the diseases such as eczema itch.Berberis Amurensis Rupr, mainly containing alkaloids such as Berberine, jateorhizine, Phellodendrine, palmatine, dauricines, separately contains obakunone, obakulactone, Dictamnolide isoreactivity composition.Berberis Amurensis Rupr Berberine content is higher, is for one of main Chinese medicinal materials starting material extracting Berberine, and also containing more rich obakulactone in Berberis Amurensis Rupr, content is about 0.5%.Utilize Berberis Amurensis Rupr to extract in the technique of Berberine at present, all separation is not carried out to obakulactone wherein and be used, thus waste a large amount of resources, very large pollution be also result in environment simultaneously.Find that be all abandoned by this part liquid in technique in the past, this not only pollutes environment, also wastes golden cypress resource greatly containing a large amount of obakulactone compositions in the waste liquid after Berberis Amurensis Rupr extraction Berberine after deliberation.And take the filtrate of suitable treatment process to separating berberine to process, and adopt macroporous adsorbent resin to carry out enriching and purifying, can effectively prepare obakulactone product.Macroporous adsorbent resin, owing to having the features such as rate of adsorption is fast, selectivity good, manipulation of regeneration is convenient, life cycle is long, is applied and is more and more applied in the extraction and isolation of herbal medicine activeconstituents.Present method carries out enzymolysis processing to from the waste liquid after Berberis Amurensis Rupr extraction Berberine, is separated, from waste liquid, obtains obakulactone in conjunction with solvent extraction with macroporous adsorbent resin.Present method can fully utilize golden cypress resource, establishes quick, efficient, the economic preparation method of the obakulactone in a golden cypress source simultaneously.
Summary of the invention
The invention provides a kind of method that waste liquid after Berberis Amurensis Rupr extraction Berberine prepares obakulactone.The method, to be separated the filtrate after obtaining crude product Berberine in ethanol extract from Berberis Amurensis Rupr for raw material, to adopt prozyme to carry out enzymolysis, is precipitated thing, refluxing extraction is carried out again with ethanol, filter to get filtrate, filtrate is carried out concentrating under reduced pressure and is reclaimed ethanol, obtains concentrated solution.Adopted by concentrated solution macroporous adsorptive resins to carry out enrichment, wash-out, obtain elutriant, elutriant is carried out concentrate, crystallization, dry, obtain obakulactone product.The obakulactone yield obtained reaches 0.35%(relative to golden cypress raw material) left and right, content reaches more than 80%.The object of the invention is to be achieved through the following technical solutions.It comprises the steps: (1) carries out enzymolysis processing to from the filtrate after Berberis Amurensis Rupr extraction Berberine: raw material: to be separated the filtrate after obtaining crude product Berberine from Berberis Amurensis Rupr ethanol extract, regulate filtrate pH value to slightly acidic with ammoniacal liquor, heating keeps temperature 50 C, the prozyme of 0.5% is added in filtrate, enzymolysis 30 minutes, be warming up to 90 DEG C, allow enzyme deactivation.Be precipitated thing.(2) alcohol reflux: after the throw out obtained is separated, adds alcohol reflux, extracted rear filtration, obtained filtrate, filtrate reduced in volume is become concentrated solution.(3) macroporous adsorbent resin is separated, and selects low-pole or nonpolar macroporous adsorption resin as D101, AB-8, resin is carried out pre-treatment, fully swelling, removal wherein contained unpolymerized organic solvent.Be seated in by macroporous adsorbent resin in glass column or stainless steel pillar, by concentrated solution wet method loading, thin-layer chromatography detects obakulactone content in effluent liquid simultaneously, and resin is until adsorb saturated.To adsorbing the distilled water of saturated macroporous adsorptive resins with 1 times of bed volume (BV) with 2 times of BV/h speed wash-outs not by the extracting solution adsorbed, then with 50% of 3BV ethanol with 2BV/h speed wash-out, collect elutriant, and then with 70% of 3BV ethanol with 2BV/h speed wash-out, collect elutriant.(4) the elutriant concentrating under reduced pressure obtained by 50% ethanol elution, crystallisation by cooling, filtration, drying, obtain obakulactone product.The obakulactone yield prepared through method of the present invention is about 0.35%, and content can reach more than 80%.In a word, advantage of the present invention is: can fully utilize the Berberis Amurensis Rupr resource extracting Berberine.Adopt prozyme to process the waste liquid after separating berberine, effectively raise the content of obakulactone.The present invention adopts macroporous adsorbent resin isolation technique to prepare obakulactone, and separation efficiency is high, does not use noxious solvent, is the extraction process of environmental protection, and preparation technology is simple, and cost is low, and quality product is high.The present invention utilizes discarded resource to carry out the preparation of obakulactone, both effectively make use of resource, has opened up a kind of new material resources, has saved resource and cost.
Embodiment
Embodiment 1
The waste liquid obtained after separating berberine from the extracting solution of Berberis Amurensis Rupr extraction Berberine to adopt ethanol extraction method is for raw material, measure waste liquid 10L, regulate filtrate pH value to about 5-7 with ammoniacal liquor, heating adds the prozyme of 50g, enzymolysis 30 minutes about keeping temperature 50 C in filtrate, be warming up to 90 DEG C, allow enzyme deactivation, natural subsidence 5-10 hour, is precipitated thing.After the throw out obtained is separated, adds 5-8 times of volume ethanol refluxing extraction, extracted rear filtration, obtained filtrate, by filtrate reduced in volume to 200mL.Select D101 macroporous adsorbent resin, resin is carried out pre-treatment, fully swelling, removal wherein contained unpolymerized organic solvent.Be seated in by the macroporous adsorbent resin of 500mL volume in glass column or stainless steel pillar, by 200mL concentrated solution wet method loading, thin-layer chromatography detects obakulactone content in effluent liquid simultaneously, until adsorb saturated.To the distilled water of the saturated macroporous adsorptive resins 200mL of absorption with 400mL/h speed wash-out not by the upper prop liquid adsorbed, then use the ethanol of 50% of 600mL volume with 400mL/h speed wash-out, collect elutriant, and then with 70% of 3BV ethanol with 2BV/h speed wash-out, collect elutriant.The elutriant that 50% ethanol elution obtains is evaporated to about 100mL, crystallisation by cooling 12h, crystal is filtered, dry, obtain obakulactone product.Obtaining obakulactone amount is about 30g, and content is 80.5%.
Embodiment 2
The waste liquid obtained after separating berberine from the extracting solution of Berberis Amurensis Rupr extraction Berberine to adopt ethanol extraction method is for raw material, measure waste liquid 100L, first be evaporated to 20L, regulate filtrate pH value to about 5-7, about heating keeps temperature 50 C with ammoniacal liquor, the prozyme of 0.1 % is added in filtrate, enzymolysis 30 minutes, is warming up to 90 DEG C, allows enzyme deactivation, natural subsidence 5-10 hour, is precipitated thing about 800g.After the throw out obtained is separated, adds the alcohol reflux of 5-8 times of liquid ratio, extracted rear filtration, obtained filtrate, filtrate reduced in volume is become to about 1000mL.Select the AB-8 macroporous adsorbent resin that pre-treatment is good, be seated in by the macroporous adsorbent resin of 2000mL volume in glass column or stainless steel pillar, by 1000mL concentrated solution wet method loading, thin-layer chromatography detects obakulactone content in effluent liquid simultaneously, until adsorb saturated.To the distilled water of the saturated macroporous adsorptive resins 1000mL of absorption with 4L/h speed wash-out not by the extracting solution adsorbed, then use the ethanol of 50% of 3L volume with 2L/h speed wash-out, collect elutriant, and then with 70% of 3BV ethanol with 2BV/h speed wash-out, collect elutriant.The elutriant that 50% ethanol elution obtains is evaporated to about 1000mL, crystallisation by cooling 12h, crystal is filtered, dry, obtain obakulactone product.Obakulactone amount is about 300g, and content is 81%.
Claims (5)
1. the method preparing obakulactone from the ethanol waste liquid after Berberis Amurensis Rupr extraction Berberine is characterized in that: comprise the following steps (1) and carry out enzymolysis processing to from the ethanol waste liquid after Berberis Amurensis Rupr extraction Berberine: to be separated the waste liquid after obtaining crude product Berberine for raw material from Berberis Amurensis Rupr ethanol extract, regulate filtrate pH value to slightly acidic with ammoniacal liquor, heating keeps temperature 50 C, the prozyme of 0.5 % is added in filtrate, enzymolysis 30 minutes, be warming up to 90 DEG C, allow enzyme deactivation, sedimentation, is precipitated thing; (2) alcohol reflux: after the throw out obtained is separated, adds alcohol reflux, extracted rear filtration, obtained filtrate, filtrate reduced in volume is become concentrated solution; (3) macroporous adsorbent resin is separated, and selects low-pole or middle polarity macroporous adsorbent resin to be separated concentrated solution, adopts the ethanol of different concns to carry out wash-out, collect obakulactone elution fractions, elutriant is concentrated, cooling, crystallization, filtration, drying, obtain obakulactone product.
2. prepare the method for obakulactone from the waste liquid after Berberis Amurensis Rupr extraction Berberine for one kind, it is characterized in that step (1), to the enzymolysis extracting the filtrate after Berberine from Berberis Amurensis Rupr, under weakness condition, temperature 45-55 DEG C, add the prozyme of 0.4-0.8 %, after enzymolysis 20-40 minute, heating makes enzyme deactivation.
3. prepare a method for obakulactone from the waste liquid after Berberis Amurensis Rupr extraction Berberine, it is characterized in that step (2) and (3), comprise the steps: alcohol reflux obakulactone; Macroporous adsorbent resin is separated obakulactone.
4. a kind of waste liquid after Berberis Amurensis Rupr extraction Berberine according to claim 3 prepares the method for obakulactone, it is characterized in that, alcohol reflux obakulactone: the throw out obtained by enzymolysis carries out alcohol reflux, add 5-10 volume ethanol doubly, refluxing extraction 1-2 hour, obtain filtrate after filtration, decompression recycling ethanol, obtains concentrated solution.
5. a kind of waste liquid after Berberis Amurensis Rupr extraction Berberine according to claim 3 prepares the method for obakulactone, it is characterized in that, macroporous adsorbent resin is separated obakulactone: the concentrated solution low-pole of upper step or the macroporous adsorbent resin of middle polarity are adsorbed, different concentration ethanol carries out wash-out, the content of obakulactone in thin-layer chromatography tracing detection effluent liquid, the obakulactone section elutriant collected is merged, concentration and recovery ethanol, crystallization, obtain obakulactone precipitation, centrifugal, dry, obtain obakulactone product.
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| CN201410481959.1A CN104262452A (en) | 2014-09-22 | 2014-09-22 | Method for preparing obakulactone from waste liquid of extracting berberine from phellodendron bark |
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| CN201410481959.1A CN104262452A (en) | 2014-09-22 | 2014-09-22 | Method for preparing obakulactone from waste liquid of extracting berberine from phellodendron bark |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108503683A (en) * | 2018-04-03 | 2018-09-07 | 重庆汇达柠檬科技集团有限公司 | A kind of method that HPMC precipitations assist limonin in reverse micelle extraction lemon seed |
| CN113827522A (en) * | 2021-10-18 | 2021-12-24 | 山东花物堂生物科技有限公司 | A cortex Phellodendri extract for cosmetic and its preparation method |
-
2014
- 2014-09-22 CN CN201410481959.1A patent/CN104262452A/en active Pending
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| 廉莲等: "川黄柏的化学成分研究", 《中国实验方剂学杂志》 * |
| 张子龙等: "关黄柏、黄柏及其精制提取物HPLC指纹图谱的相关性研究", 《中药新药与临床药理》 * |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108503683A (en) * | 2018-04-03 | 2018-09-07 | 重庆汇达柠檬科技集团有限公司 | A kind of method that HPMC precipitations assist limonin in reverse micelle extraction lemon seed |
| CN108503683B (en) * | 2018-04-03 | 2020-11-10 | 重庆汇达生物科技股份有限公司 | Method for extracting limonin from lemon seeds by HPMC precipitation-assisted reverse micelle |
| CN113827522A (en) * | 2021-10-18 | 2021-12-24 | 山东花物堂生物科技有限公司 | A cortex Phellodendri extract for cosmetic and its preparation method |
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Application publication date: 20150107 |