CN1334269A - Process for extracitng puerarin from waste water from producing puerarin starch and increasing its yield - Google Patents
Process for extracitng puerarin from waste water from producing puerarin starch and increasing its yield Download PDFInfo
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Abstract
A process for extracting the puerarin from the waste water from production of pueraria starch with high yield includes choosing macroporous adsorption resin which has both adsorption and catalytic conversion functions, making said waste water flow through the chromatographic column of said resin or mixing it with said resin, eluting the adsorbed and converted puerarin with organic solvent, and vacuum recovery of said solvent. Its advantages are use of waste, low cost and environmental production.
Description
The present invention relates to a kind of method of extracting puerarin and improving its output, particularly a kind of method of from the waste water of producing kudzuvine root starch, extracting puerarin and improving its output.
The Chinese medicine root of kudzu vine is the root of legume pueraria lobata (pueraria Lobata wild ohwi) or Pachyrhizua angulatus (p.thomsonii Benth).Widely distributed in China, aboundresources.It contains more starch and isoflavone like substance, can dietotherapeutic.Kudzuvine root starch is the protective foods of China's folk tradition.With the puerarin is the isoflavone like substance of main component, is commonly referred to as Radix Puerariae flavone, has multiple pharmacologically active, has become the active drug of treatment diseases of cardiovascular and cerebrovascular systems.Radix Puerariae flavone is made up of multiple isoflavonoid, except that the major ingredient puerarin, the derivative that also has puerarin, as 3 '-methoxy puerarin, 7-xylosyl puerarin, 4 ', 6 ' one diacetyl puerarins, they can be converted into puerarin under certain condition, in addition, also have Daidzin, daidzein, 4, (1. Jun-ei kinjo.et al.Chem Pharm Bull such as 7-glucosulfone Daidzin, 1987,35 (12): 4846; Chinese Medical Journal, 1974,54 (5): 271) such as 2. just leave.In recent years, because pueraria starch, Radix Puerariae flavone at home and abroad are in great demand on the market day by day, kudzuvine root starch factory has been built up in many roots of kudzu vine place of production, but owing to technology and fund reason, usually can only therefrom extract starch, the Radix Puerariae flavone class material that a large amount of value are higher is but white from running off with factory effluent.Because it is big to extract the kudzuvine root starch water consumption, it is very low to contain Radix Puerariae flavone concentration in the waste water, with general chemical process it is extracted difficulty and proves effective.For this reason, we have invented the method for extracting Radix Puerariae flavone from the waste water of producing kudzuvine root starch, and have applied for patent.In the research experiment that continues, we have invented a kind of method of extracting and improving puerarin output, and not seeing as yet so far has this report both at home and abroad.
Purpose of the present invention just provide a kind of in producing the waste water of kudzuvine root starch (hereinafter to be referred as waste water) extract with macroporous adsorbent resin and the method for catalyzed conversion, volume increase puerarin.
The present invention can realize in the following manner: with macroporous adsorbent resin the waste water of producing kudzuvine root starch is carried out adsorption catalysis and transform, the waste water pH value is 4～6, by the puerarin of absorption with macroporous adsorbent resin and conversion, obtain thick puerarin behind the recovery organic solvent with the organic solvent wash-out.The waste water of the producing kudzuvine root starch macroporous adsorption resin chromatography post of flowing through carries out adsorption catalysis and transforms.Perhaps macroporous adsorbent resin is put into the waste water of producing kudzuvine root starch, shakes and adsorbs and catalyzed conversion in 1～2 hour, separates macroporous adsorbent resin and is adsorbed the waste water that transformed.Macroporous adsorbent resin is NKA-9, LD605.With the standard substance puerarin for to measure content of puerarin to impinging upon on the 752 ultraviolet grating spectrophotometers.The waste water of producing kudzuvine root starch comprises that the root of elegant jessamine, Pachyrhizua angulatus and high eyebrow Pueraria lobota (pueraria omeiensis) plant is that raw material extracts the waste water that kudzuvine root starch produced or the aqueous solution of their aqueous extract or their extract, and organic solvent is 90～95% edible ethanol or 50% edible ethanol.
The present invention has utilized the waste water of kudzuvine root starch manufacturer, extracts and the volume increase puerarin, has improved the utilization ratio of root of kudzu vine resource, has reduced production cost, and has avoided the pollution of waste water to environment.
The schedule of operation of the inventive method is as follows:
1, macroporous adsorbent resin is handled by medicine use standard: elder generation was with distilled water immersion 48 hours and remove solid impurity, use 2MOL NaOH solution soaking 4 hours again, be washed to neutrality, then use 2MOL HCl solution soaking 8 hours, be washed to neutrality, till being washed till a small amount of pure washing lotion and adding water and white casse do not occur with 95% edible ethanol again, washing eluting water liquid at last with water does not have till the alcohol flavor.
2, the detection of puerarin
1., the drafting of typical curve: (Nat'l Pharmaceutical ﹠ Biological Products Control Institute provides chemical reference substance to the puerarin standard specimen, the mensuration of gradient concentration 753-200007) and corresponding uv-absorbing; Add the 5mg puerarin in the 25ml volumetric flask, with dissolving of 95% edible ethanol and constant volume, accurate absorption 0.2,0.4,0.6,0.8,1.0ml are in the 10ml volumetric flask, add 4ml95% ethanol respectively, utilize water to be settled to 10ml more respectively, shake up, with same solvent is blank, measure the ultraviolet absorptivity of each concentration at 250nm wavelength place, in this interval, puerarin concentration and corresponding ultraviolet absorptivity are linear, are ordinate with the optical density, are that abscissa is made typical curve with concentration (mg/ml).Regression equation is: Y=0.075+43.35X r=0.9989 (y represents ultraviolet absorptivity, and x represents puerarin concentration).
2., measure puerarin content: the ultraviolet absorptivity of puerarins such as the original waste water before adsorbing with 752 ultraviolet grating spectrophotometric determinations, the waste water after the absorption, elutriant, find out the concentration of corresponding puerarin from typical curve, calculate content and macroporous adsorbent resin elution amount, extraction yield, inversion quantity, transformation efficiency, units increased in production, stimulation ratio puerarin.
Eluting rate=elution amount/adsorptive capacity * 100%
Original content * 100% in extraction yield=elution amount/test solution
Residual quantity+elution amount-waste water Central Plains content in the waste water of inversion quantity=be adsorbed
Transformation efficiency=inversion quantity/waste water Central Plains content * 100%
Units increased in production=elution amount-raw wastewater Central Plains content
Stimulation ratio=units increased in production/waste water Central Plains content * 100%
3, measure the pH value of the waste water solution that contains puerarin, pH value is 4～6.
4, absorption, transform: in the macroporous adsorbent resin filling chromatography column of handling well, make the waste water that contains puerarin and derivative thereof after the filtration chromatography column of flowing through, puerarin and derivative thereof are attracted on the resin, and carry out catalyzed conversion; Or macroporous adsorbent resin put in the waste water solution that contains puerarin and derivative thereof, shake absorption 1～2 hour, puerarin and derivative thereof are adsorbed on the resin, and carry out catalyzed conversion, filter, with resin and water sepn.
5, wash-out desorb: by absorption with macroporous adsorbent resin and the puerarin that transforms, or with 50% edible ethanol wash-out, the decompression recycling ethanol elutriant obtains thick puerarin with 90～95% edible ethanol wash-out desorbs.With embodiment in detail it is described in detail.
Embodiment one
Take by weighing the wet basis macroporous adsorbent resin NKA-93g (dry weight 0.9g) and the LD605 2g (dry weight 0.7g) that have handled well respectively, load in the glass chromatography column of 2 40cm * 1.4cm sample introduction behind the watering balance respectively.Measure the waste water of 2 parts of each 20ml, this waste water is taken from Suizhou City flood mountain, Hubei Province kudzuvine root starch factory, system is obtained by the Radix Puerariae when real estate, pH value 4, containing Radix Puerariae flavone concentration is 1.08mg/ml, allow the chromatography column of its above-mentioned 2 kinds of macroporous adsorbent resins of flowing through respectively, control take-off rate be 3-5 drip/minute, effluent liquid is 3 resin columns of flowing through repeatedly, after operation is finished, the puerarin that the NKA-9 resin column is obtained by the puerarin of resin absorption and catalyzed conversion puerarin derivate with 20ml95% edible ethanol wash-out repeats wash-out and makes for 3 times ethanol eluate not contain puerarin (UV spectrophotometer measuring), and the ethanol eluate constant volume is 80ml and dilutes 20 times; Through exhausted water constant volume 20ml behind resin column absorption and the catalyzed conversion and be diluted to 10 times; Be that blank is measured the two ultraviolet absorptivity at 250nm wavelength place with the edible ethanol of water and 95% respectively with 752 ultraviolet grating spectrophotometers again.From the puerarin typical curve, find ethanol eluate respectively and by the puerarin concentration resin absorption and the exhausted water that transformed, calculate the elution amount, extraction yield, inversion quantity, transformation efficiency, units increased in production, stimulation ratio of 2 kinds of resins etc. again.The test operation of LD605 resin column is fully with the NKA-9 resin column, and what its difference only was that eluting solvent uses is 50% edible ethanol, and various data see table one for details, the decompression recycling ethanol elutriant obtains thick puerarin.
Table one column chromatography extracts and transforms the puerarin in the waste water
| The resin title | NKA-9 | ?LD605 |
| Waste water Central Plains content mg/20ml | 21.6 | ?27.6 |
| Concentration mg/1ml in the ethanol eluate | 1.387 | ?1.55 |
| Elution amount mg | 27.74 | ?31 |
| Extraction yield % | 128.42 | ?112.32 |
| Inversion quantity mg | 6.54 | ?3.9 |
| Transformation efficiency % | 30.27 | ?14.13 |
| Units increased in production mg | 6.14 | ?3.4 |
| Stimulation ratio % | 28.42 | ?12.32 |
Find out that from the data of table one NKA-9 and LD605 resin extract, transform puerarin in the waste water and derivative thereof in the column chromatography mode, effect of increasing production is obvious.The extraction yield of NKA-9 resin column is 128.42%, and transformation efficiency is 30.27%, and stimulation ratio is 28.42%, and the extraction yield of LD605 resin column is 112.32%, and transformation efficiency is 14.13%, and stimulation ratio is 12.32%; The two compares, and the effect of the extraction catalyzed conversion of NKA-9 resin and volume increase is more excellent.
Embodiment two
Take by weighing 1.5g NKA-9 wet basis macroporous adsorbent resin and 1.5g LD605 macroporous adsorbent resin respectively, put into triangular flask, adding 10ml puerarin concentration in the former triangular flask is the waste water (wastewater source is with embodiment one) of 1.23mg/1ml, pH value 6, adding 10ml puerarin concentration in latter's triangular flask is the waste water of 0.792mg/1ml, pH value 6.The two all is placed on and shakes absorption and catalyzed conversion on the shaking table, the former shook 1 hour, the latter 2 hours, filtering separation resin and absorption, the waste water that transformed, resin is put in the triangular flask, the former adds 90% edible ethanol 10ml, and the latter adds 50% edible ethanol 10ml, shakes wash-out 1 hour, repeat 2 times, merge elutriant respectively, and be settled to 40ml, dilute 20 times; Waste water through absorption and catalyzed conversion is settled to 20ml, dilutes 5 times; Measure ethanol eluate and the optical density of adsorbing puerarin in the waste water that transformed at 250nm wavelength place with ultraviolet spectrophotometry respectively, on the puerarin typical curve, find corresponding puerarin concentration.Eluted puerarin concentration that Here it is transforms residual puerarin concentration in the waste water of back with absorption, calculates each related data then, sees table two for details, and the decompression recycling ethanol elutriant obtains thick puerarin.
Table two shakes absorption method the puerarin in the waste water is extracted and transforms
| The resin title | ?NKA-9 | ?LD605 |
| Waste water Central Plains content mg/10ml | ?12.3 | ?7.92 |
| Concentration mg/1ml in the ethanol eluate | ?1.53 | ?0.86 |
| Elution amount mg | ?15.3 | ?8.6 |
| Extraction yield % | ?124.4 | ?108.6 |
| Inversion quantity mg | ?3.19 | ?0.74 |
| Transformation efficiency % | ?25.93 | ?9.3 |
| Units increased in production mg | ?3 | ?0.68 |
| Stimulation ratio % | ?24.39 | ?8.6 |
Find out that from table two NKA-9 and LD605 resin in shaking puerarin are adsorbed and to the puerarin derivate catalyzed conversion, its effect difference is bigger, it is remarkable that NKA-9 resin and volume increase transform the extraction action effect, transformation efficiency reaches 25.93%, and stimulation ratio reaches 24.39%, extraction rate reached 124.39%.The effect of LD605 resin is then relatively poor; If compare with the column chromatography mode of embodiment one, not only aspect absorption and changing effect, and operate convenient aspect, the column chromatography mode is all superior than the mode of shaking.Extract the test-results that transforms and increase production puerarin with our macroporous adsorbent resin of screening in the mode of shaking, prove that again this macroporous adsorbent resin has the function that the catalyzed conversion puerarin derivate is a puerarin.
Claims (10)
1, from the waste water of producing kudzuvine root starch, extracts puerarin and improve the method for its output, it is characterized in that with macroporous adsorbent resin the waste water of producing kudzuvine root starch being carried out adsorption catalysis transforms, the waste water pH value is 4-6, by the puerarin of resin absorption and conversion, obtain thick puerarin behind the recovery organic solvent with the organic solvent wash-out.
2, according to the described extraction puerarin of claim 1 and improve the method for its output, the waste water that it is characterized in that producing kudzuvine root starch is flowed through, and the macroporous adsorption resin chromatography post adsorbs, catalyzed conversion.
3, according to the described extraction puerarin of claim 1 and improve the method for its output, it is characterized in that macroporous adsorbent resin puts into the waste water of producing kudzuvine root starch, shake and adsorbed and catalyzed conversion in 1-2 hour, separate macroporous adsorbent resin and be adsorbed the waste water that transformed.
4,, it is characterized in that macroporous adsorbent resin is NKA-9 according to the described extraction puerarin of claim 1 and improve the method for its output.
5,, it is characterized in that macroporous adsorbent resin is LD605 according to the described extraction puerarin of claim 1 and improve the method for its output.
6, according to the described extraction puerarin of claim 1 and improve the method for its output, the waste water that it is characterized in that producing kudzuvine root starch is that the root of elegant jessamine, Pachyrhizua angulatus, delicate eyebrows Pueraria lobota is the waste water that the raw material production kudzuvine root starch is produced.
7, according to the described extraction puerarin of claim 1 and improve the method for its output, the waste water that it is characterized in that producing kudzuvine root starch is that the root of elegant jessamine, Pachyrhizua angulatus, delicate eyebrows Pueraria lobota is the aqueous extract of raw material.
8, according to the described extraction puerarin of claim 1 and improve the method for its output, the waste water that it is characterized in that producing kudzuvine root starch is that the root of elegant jessamine, Pachyrhizua angulatus, delicate eyebrows Pueraria lobota is the aqueous solution of the crude extract of raw material.
9,, it is characterized in that organic solvent is the edible ethanol of 90-95% according to the described extraction puerarin of claim 1 and improve the method for its output.
10,, it is characterized in that organic solvent is 50% edible ethanol according to the described extraction puerarin of claim 1 and improve the method for its output.
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| CNB011276223A CN1176934C (en) | 2001-07-11 | 2001-07-11 | Process for extracitng puerarin from waste water from producing puerarin starch and increasing its yield |
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| CNB011276223A CN1176934C (en) | 2001-07-11 | 2001-07-11 | Process for extracitng puerarin from waste water from producing puerarin starch and increasing its yield |
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| CN1176934C CN1176934C (en) | 2004-11-24 |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936242A (en) * | 2012-11-28 | 2013-02-20 | 云南省农业科学院药用植物研究所 | Method for comprehensively utilizing arrowroot |
| CN107522692A (en) * | 2017-10-25 | 2017-12-29 | 贵州国农葛业有限公司 | A kind of method that waste liquid separating puerarin is produced using pueraria starch |
| CN108014169A (en) * | 2016-11-03 | 2018-05-11 | 西南大学 | A kind of preparation method and applications of kudzu root extract and/or kudzu root flavone |
| WO2018171117A1 (en) * | 2017-03-23 | 2018-09-27 | 苏州顶裕节能设备有限公司 | Shampoo prepared with kudzu powder waste water and method therefor |
| CN108685061A (en) * | 2017-04-12 | 2018-10-23 | 西南大学 | A kind of pueraria lobata ultramicro whole powder and the composition comprising it and application |
| CN112679562A (en) * | 2020-12-30 | 2021-04-20 | 江西农业大学 | A method for preparing puerarin by macroporous resin method |
-
2001
- 2001-07-11 CN CNB011276223A patent/CN1176934C/en not_active Expired - Fee Related
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102936242A (en) * | 2012-11-28 | 2013-02-20 | 云南省农业科学院药用植物研究所 | Method for comprehensively utilizing arrowroot |
| CN108014169A (en) * | 2016-11-03 | 2018-05-11 | 西南大学 | A kind of preparation method and applications of kudzu root extract and/or kudzu root flavone |
| WO2018171117A1 (en) * | 2017-03-23 | 2018-09-27 | 苏州顶裕节能设备有限公司 | Shampoo prepared with kudzu powder waste water and method therefor |
| CN108685061A (en) * | 2017-04-12 | 2018-10-23 | 西南大学 | A kind of pueraria lobata ultramicro whole powder and the composition comprising it and application |
| CN107522692A (en) * | 2017-10-25 | 2017-12-29 | 贵州国农葛业有限公司 | A kind of method that waste liquid separating puerarin is produced using pueraria starch |
| CN112679562A (en) * | 2020-12-30 | 2021-04-20 | 江西农业大学 | A method for preparing puerarin by macroporous resin method |
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| CN1176934C (en) | 2004-11-24 |
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