CN104177863B - A kind of method extracting haematochrome from green pine needle - Google Patents
A kind of method extracting haematochrome from green pine needle Download PDFInfo
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Abstract
The invention discloses a kind of method extracting haematochrome from green pine needle.The method adopts the green pine needle of 1% methanol hydrochloride solution or 1% ethanol solution hydrochloride lixiviate to obtain reddish-brown vat liquor, then adds alkali precipitation, and the red-purple powder obtained after centrifugal, drying, is pine needle haematochrome raw product.Prove through overtesting, the pine needle haematochrome that the present invention extracts is the mixture of high polymerization pycnogenols and cyanidin(e) and derivative thereof.The present invention proves that red height polymerization pycnogenols and cyanidin(e) produce in leaching process, this makes the output of pine needle haematochrome significantly improve, and simultaneously a large amount of productions of pine needle haematochrome are increase pine needle liquor color, improve pine needle tea quality and provide a kind of feasible selection.Present method is simple and practical, with low cost, is suitable for industrial a large amount of production.
Description
Technical field
The present invention relates to a kind of method for extracting pigment, relate in particular to a kind of method extracting haematochrome from green pine needle.
Background technology
Pigment miscellaneous is extensively there is, as cyanidin(e) (Chalker-Scott, 2002 among plant organ especially petal, pericarp, tender leaf and fall foliage; Fieldetal., 2001; Gouldetal., 1995; ZhangandWang, 2008).And the redness in many fruits usually becomes raw material and the additive of food-processing industry and medicine industry.In related products, domestic invention and the report (Xiao Weixiang etc., 1987,1997) once having thearubigins.Pine needle tea has merchandise sales as a kind of special health promoting beverage, but soup colour cast is light.Pine needle green in the evergreen needle of pine tree, the especially season of growth, haematochrome content is very little, and colourless pycnogenols (catechin and derivative thereof) content is higher.The pycnogenols of common pinaceae plant has obvious anti-oxidant activity and antitumour activity (Huang Qiliang, 2012; Wang Qiuyue etc., 2009).Therefore, the extraction process of Pine Procyanidins becomes one of production and processing technology of people's concern.Research in the past shows, Pine Procyanidins extracts (Wang Qiuyue etc., 2009) mostly from the bark of pine tree.For pine needle, pine bark resource quantity is less, especially strips off the skin from standing tree comparatively inconvenient.Although there is the report (Huang Qiliang, 2012) extracting pycnogenols from pine needle, from fresh green pine needle, the technique of extracting directly haematochrome has no report.
The present inventor finds that in the process using hydrochloric acid methanol (or acidic alcohol) lixiviate pine needle colourless pycnogenols oxypolymerization forms red polymerization pycnogenols and cyanidin(e) (Cyanidin-3-O-glucoside etc.), thus constantly has the mixture of haematochrome to be leached out.The method of extraction pycnogenols conventional is at present extracted mostly from the fruits such as grape, and output is by the impact in season, and the biennial bearing produced by fruit affects.For other organ, pine needle stock number is comparatively large, and season of growth appropriateness gather pine needle to the growth of pine tree and Survival Effects little, this creates conditions for a large amount of pine needle haematochrome of producing.
Summary of the invention
The object of the invention is to seek a kind of method that can improve extraction pine needle haematochrome efficiency, for round-the-clock, production in enormous quantities pine needle haematochrome lay the foundation.
Technical scheme of the present invention is: a kind of method extracting haematochrome from green pine needle, it is characterized in that, adopt the green pine needle of 1% methanol hydrochloride solution lixiviate to obtain reddish-brown vat liquor, then add alkali precipitation, the red-purple powder obtained after centrifugal, drying, is pine needle haematochrome raw product.
Specifically comprise the following steps:
(1) take middle age or the biennial above green pine needle of maturity age pine tree, naturally dry after cleaning; Then stand-by after dry and soft for green pin being cut into segment;
(2) dry and soft for green pin and 1% methanol hydrochloride solution are added in leaching vessel, lixiviate 16-18 hour under indoor nature temperature, and pour out vat liquor (abandoning) when pine needle surface has been adsorbed a large amount of haematochrome and become red-brown;
(3) add the red pigments that 1% methanol hydrochloride solution wash-out is adsorbed on the positions such as pine needle surface again, constantly stir to improve extraction efficiency, continue lixiviate 70-100 hour, pour out reddish-brown vat liquor stand-by; Add 1% methanol hydrochloride solution again among leaching vessel, continue lixiviate 70-100 hour; Stand-by by mixing after above-mentioned twice vat liquor filtration residue or centrifugal removing impurity;
(4) reddish-brown extracted toward step (3) is extracted in stoste and is added NaOH, adjustment solution ph is to 12-14, change into after purple Precipitation completely until red pigments, the red-purple powder obtained after centrifugal, drying, is pine needle haematochrome raw product.
In said extracted method, divide and add 1% methanol hydrochloride solution three times, preferably, 1% methanol hydrochloride solution added for the 1st, 2,3 time and the mass ratio of the dry and soft pin of green are 12-20:12-20:12-20:1, and optimum ratio is 16:16:16:1.The compound method of 1% methanol hydrochloride solution is: the concentration of 2.77ml be 36.5% hydrochloric acid add methanol constant volume to 100ml.
Preferably add the 1M sodium hydroxide that reddish-brown extracts stoste volume 1/13 in above-mentioned steps (4), adjust ph is 13.
Centrifugal in above-mentioned steps (4), be preferably 8000 revs/min centrifugal 10 minutes.
Apply the hydrochloric acid methanol that 1% acidic alcohol substitutes 1% in said extracted method and can obtain pine needle haematochrome equally, and harmless with extraction using alcohol, but haematochrome extracted amount slightly difference.
Water distilling apparatus can be applied in said extracted method and reclaim the discarded methyl alcohol of said process.
Prove through overtesting, the pine needle haematochrome that the present invention extracts is the mixture of high polymerization pycnogenols and cyanidin(e) and derivative thereof.This mixture is mainly water colo(u)r, in bluish voilet in alkaline environment, in red-brown under sour environment.
Application: add in pine needle tea, increases pine needle liquor color, can also be used as food or drug additive.
The present invention is proved by experimental study, and this technique can extract red pigments from green pine needle, and improves the extracted amount of haematochrome along with the increase of drying treatment degree.Present method utilizes the principle of pine needle cuticular macromole fatty acid ester absorption red pigments, by extraction reasonable in design and elution process, serves the effect of macromolecules adsorption resin method purification pigment.Method is simple, convenient, practical, and with low cost, is suitable for industrial a large amount of production pine needle haematochrome.The extraction yield of haematochrome (in fresh pine needle) between 5%-8% by analysis, if select the technique extraction yield of suitable pine needle material and optimization to bring up to 10%-18%.
Because pine needle output is large, evergreen all the year round, extract haematochrome substantially by stock number with seasonally to affect from pine needle.The present invention proves that red height polymerization pycnogenols and cyanidin(e) produce in leaching process, and this makes the output of pine needle haematochrome significantly improve, and even exceedes bark.A large amount of productions of pine needle haematochrome are increase pine needle liquor color, improve pine needle tea quality and provide a kind of feasible selection.Present method is simple and practical, with low cost, is suitable for industrial a large amount of production.
Accompanying drawing explanation
Fig. 1 is with the microscopic examination of haematochrome generating unit during methanol hydrochloride solution lixiviate pine needle and the change of vat liquor color; A. hydrochloric acid methanol lixiviate pine needle horny layer of epidermis change after 24 hours, finds that there is anthocyanin and is formed; B. hydrochloric acid methanol lixiviate changed in pine needle endodermis after 24 hours, found that there is the formation of anthocyanin; C. hydrochloric acid methanol: the lixiviate of water (50%:50%) mixed solution is pine needle horny layer of epidermis and endodermis change after 24 hours, finds the formation without obvious anthocyanin of pine needle horny layer of epidermis and endodermis; D. the hydrochloric acid methanol lixiviate extracting solution color of 8 hours, extracting solution is green; E. the hydrochloric acid methanol lixiviate extracting solution color of 120 hours, extracting solution is red-brown;
Fig. 2 is under hydrochloric acid methanol (100%) and the miscible sequence extracting solution of acidic methanol-water (90%, 80%, 70% and 50%) lixiviate, the trend that vat liquor changes with extraction time at 525nm wave band absorbance;
Fig. 3 is the change of haematochrome extracted amount in hydrochloric acid methanol and the miscible extracting solution of methanol-water; A. under hydrochloric acid methanol (100%) and the miscible sequence extracting solution of methanol-water (95%, 90%, 85%) lixiviate, in the variation tendency of 525nm wave band absorbancy.B. under hydrochloric acid methanol (100%) and the miscible sequence extracting solution of methanol-water (98.75%, 97.5%, 96.26%, 95%) lixiviate, in the variation tendency of 525nm wave band absorbancy;
Fig. 4 is the difference of haematochrome extracted amount after pine needle dehydration and rehydration; A. the correlationship of water content and the hydrochloric acid methanol extracting solution OD value under 525nm after pine needle drying and dehydrating; B. the pine needle of dry dehydration soak once again after the OD of anthocyanin extracting solution
525/645value compares; Wherein CK be normal pine needle in contrast, Rw is the needle of rehydration again after dehydration;
Fig. 5 is the contrast of anthocyanin extracted amount of the fresh needle of black pine, dry needle, then needle, for many years needle, Pollen pini thunbergii bark and Japanese red pine skin;
Fig. 6 is pine needle and bark extracting solution and sedimentary RGB image analysis; A. the G/R value of pine needle pigment powder redissolution thing (L-n), bark pigment powder redissolution thing (P-n), pine needle extract (L-o), bark extracting solution (P-o), pine needle throw out (L-d) and bark deposits thing (P-d) image; The B/R value of image shown in b.a;
Fig. 7 is pycnogenols and cyanidin(e) main component high performance liquid chromatography wave spectrogram picture; A. the wave spectrogram picture of pycnogenols elementary cell composition (catechin); B. the wave spectrogram picture of cyanidin(e) elementary cell composition (Cyanidin-3-O-glucoside);
Fig. 8 is the process flow sheet that the embodiment of the present invention 4 extracts red pigments from green pine needle.
Embodiment
The impact on extraction effect such as the water content of embodiment 1 extraction time and extracting solution
The present invention adopts 1% hydrochloric acid methanol to extract black pine (PinusthunbergiiParl.) pine needle haematochrome.Research finds, during with hydrochloric acid methanol lixiviate black pine pine needle, based on green pigment in beginning vat liquor, does not almost have haematochrome to extract (within 5 hours) (Fig. 1 d).Along with the prolongation of extraction time, in methanol hydrochloride solution, also gradually change into yellow-green colour by blue green.On pine needle surface, (Fig. 1 a) He in endodermis cell (Fig. 1 b) engenders red pigments, and the haematochrome at this moment produced is attracted to above cuticular macromole fatty acid ester mostly.Continuation with extraction time extends, and becomes red-brown (Fig. 1 e) along with the chlorophyll content extracted decomposition under light illumination (Fengetal., 2009) extracting solution through red-purple.In normal room temperature environment, complete and extract between needs 300 to 400 hours.This leaching process is influenced by environmental temperature, heats and can shorten extraction time and the progress of quickening extraction.In order to save extraction cost, the present invention only extracts under natural room temperature.By contrast, form (Fig. 1 c) without obvious haematochrome during use 50%:50% hydrochloric acid methanol-water mixed liquid body (Gong etc. 2004) lixiviate and almost do not have haematochrome to be extracted.
The absorbancy using visible spectrophotometer to measure the hydrochloric acid methanol extracting solution of 100% of pine needle at 525nm wave band finds, the corresponding OD value of increase along with extraction time improves gradually, until more than 300 hour just settles out (Fig. 2-100) gradually.When extracting identical pine needle in the miscible system of acidic methanol-water (10% water+90% hydrochloric acid methanol) 90% (Fig. 2-90), extracting solution at the absorbance value of 525nm wave band significantly lower than the extracting solution of the pure solution of 100% hydrochloric acid methanol.During the pine needle that in the acidic methanol-water immiscible liquid (50% water+50% hydrochloric acid methanol) 50%, extraction is identical (Fig. 2-50), extracting solution is little of being almost difficult to record out (Fig. 2-50) at the absorbance value of 525nm wave band.
Reduce further methanol-water miscible liquids gradient between 85% and 100% (Fig. 3 a), to (Fig. 3 b) between 95% and 100%, even between 99% to 100%, the trend that the increase red pigments growing amount with water content reduces still exists.Therefore, the impact of pine needle haematochrome by the water content of extracting solution is extracted with hydrochloric acid methanol.And, adopt hydrochloric acid methanol extraction pine needle haematochrome to need lasting an immersion and make pine needle oxypolymerization and change the process that colourless pycnogenols becomes haematochrome.
Embodiment 2 pine needle water ratio is on the impact of extraction effect
Fig. 4 and Fig. 5 is shown in the impact of pine needle water ratio on extraction effect, the data of Fig. 4 show, the needle haematochrome extracted amount of processed obviously increases, and between pine needle water ratio and the haematochrome absorbance of extracting solution, there is obvious linear relationship, (Fig. 4 a).The pine needle of drying treatment is again after rehydration process, and compared with not withering contrast pine needle, haematochrome extracting solution does not have the difference (Fig. 4 b) on statistical significance.
This test illustrates, be the process of an oxypolymerization gradually by the process that hydrochloric acid methanol extracts pine needle haematochrome, drying treatment pine needle is conducive to the extracted amount improving pine needle haematochrome.In addition, except drying and dehydrating can improve pine needle haematochrome extracted amount, perennial pine needle compares the haematochrome quantum of output high (Fig. 5) of newborn pine needle then.The extracted amount of pine needle haematochrome even higher than bark (Fig. 5), especially dried needle.The red pigments amount extracted from the green pine needle of drying is even higher than withered pine needle russet.
The composition analysis of embodiment 3 pine needle haematochrome
Research shows, the red solution color after alkaline sedimentation continuing the green pine needle generation of lixiviate in acidic methanol solution becomes bluish voilet (Fig. 6 a-Ld, Fig. 6 b-Ld), although the BS of bark extracting solution also has become lilac trend, its degree more much lower than pine needle (Fig. 6 a-Pd, Fig. 6 b-Pd).This points out the formation having cyanidin(e) or anthocyanin in pine needle leaching process indirectly.And pycnogenols is easy to change into cyanidin(e) under sour environment condition.
Meanwhile, the process that the present invention's hydrochloric acid methanol extracts pine needle haematochrome is the process of an oxypolymerization gradually, and colourless oligomeric procyanidolics is converted into height polymerization pycnogenols (Huang Qiliang, 2012) of reddish-brown through oxypolymerization.
In order to prove that following test is carried out in the existence of high polymerization pycnogenols and cyanidin(e) further: get 1g black pine pine needle, cut into 1mm long, insert test tube and add 1% hydrochloric acid methanol 20ml lixiviate to stable, get red extracting solution and analyze its Cyanidin-3-O-glucoside (cyanidin(e) elementary cell composition) and catechin (pycnogenols elementary cell composition), be used in conjunction analysis through high performance liquid chromatography and mass spectrum and show that in this extracting solution, existing height polymerization pycnogenols also has cyanidin(e).Fig. 7 is shown in by its wave spectrogram picture, and its assay result is as table 1.Therefore, prove that the red pigments formed in the leaching process that continues at methanol hydrochloride solution is the mixture of high polymerization pycnogenols and cyanidin(e) and derivative thereof.Apply suitable separation means and can produce the pine needle haematochrome with certain activity.
Cyanidin-3-O-glucoside in table 1 vat liquor and catechin content
| Component number | Compound title | Content/mg/L |
| 1 | Cyanidin-3-O-glucoside | ～111.05 |
| 2 | Catechin | ～857.59 |
Embodiment 4
(1) take the biennial above green pine needle of maturity age pine tree, clean surperficial floating dust; Dry under Indoor Natural environment (temperature 25-35 DEG C, relative humidity 50-70%) condition; Then stand-by after being cut into the long segment of 1mm;
(2) by 1% methanol hydrochloride solution of dry and soft for green pin and 16 times of quality (in the dry and soft pin of green) among leaching vessel, lixiviate 16-18 hour under indoor nature temperature, and pine needle surface is when having adsorbed a large amount of haematochrome and become red-brown, pours out yellow-green colour or brown vat liquor; The compound method of 1% methanol hydrochloride solution is: the concentration of 2.77ml be 36.5% hydrochloric acid add methanol constant volume to 100ml;
(3) add isopyknic 1% methanol hydrochloride solution is adsorbed on the positions such as pine needle surface red pigments for wash-out again, constantly stir to improve extraction efficiency, continue lixiviate 75 hours, to pour out reddish-brown vat liquor stand-by; Add isopyknic 1% hydrochloric acid methanol again and in leaching vessel, continue lixiviate 75 hours, mix after above-mentioned twice vat liquor filtration residue;
(4) ratio of 13:1 adds 1MNaOH in reddish-brown extraction stoste by volume, adjustment solution ph to 13, change into after purple Precipitation centrifugal 10 minutes with 8000 revs/min completely until red pigments after half an hour, outwell supernatant liquor, dried red-purple powder is pine needle haematochrome raw product; Extraction yield is 12-18%;
(5) apply water distilling apparatus and reclaim the discarded methyl alcohol of said process.
Embodiment 5
(1) take the biennial above green pine needle of middle pine tree in age, clean surperficial floating dust; Dry under Indoor Natural environment (temperature 25-35 DEG C, relative humidity 50-70%) condition; Then stand-by after being cut into the long segment of 1mm; The compound method of 1% ethanol solution hydrochloride is: the concentration of 2.77ml be 36.5% hydrochloric acid add ethanol and be settled to 100ml;
(2) by 1% ethanol solution hydrochloride of dry and soft for green pin and 18 times of quality (in the dry and soft pin of green) among leaching vessel, lixiviate 16-18 hour under indoor nature temperature, and pine needle surface is when having adsorbed a large amount of haematochrome and become red-brown, pours out yellow-green colour or brown vat liquor;
(3) add isopyknic 1% ethanol solution hydrochloride is adsorbed on the positions such as pine needle surface red pigments for wash-out again, constantly stir to improve extraction efficiency, continue lixiviate 80 hours, to pour out reddish-brown vat liquor stand-by; Add isopyknic 1% acidic alcohol again and in leaching vessel, continue lixiviate 80 hours, mix after above-mentioned twice vat liquor filtration residue;
(4) ratio of 13:1 adds 1MNaOH in reddish-brown extraction stoste by volume, adjustment solution ph to 13, change into after purple Precipitation centrifugal 10 minutes with 8000 revs/min completely until red pigments after half an hour, outwell supernatant liquor, dried red-purple powder is pine needle haematochrome raw product; Its extraction yield is 10-15%;
(5) apply water distilling apparatus and reclaim the discarded ethanol of said process.
Reference
1.Chalker-Scott,L.2002.DoanthocyaninsfunctionasosmoregulatorsinleaftissuesAdv.Bot.Res.,37:103-127.
2.Feild,T.S.,Lee,D.W.andHolbrook,N.M.,2001.WhyLeavesTurnRedinAutumn.TheRoleofAnthocyaninsinSenescingLeavesofRed-OsierDogwood.PlantPhysiol.,127:566–574.
3.FengAi-qing,HuQiu-Luan,WangRui-rui.2009.ExtractionandStabilityofChlorophyllinEuonymusjaponicus.JournalofLuoyangNormalUniversuty,28(2):75-77.
4.GongZhen,LIXiang-Yuan,LIZe-Rong.2004.Hydrogen-bondingInteractioninWater/MethanolMixedSolventandTheoreticalStudiesonSolubilityofPolymerChain.
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7. Huang opens preparation and the primary bioactivity research of bright .2012. pine needle pycnogenols. Master's thesis, Zhejiang Normal University.
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10.LiuGui-lin,DuHong-yun,WandYan,LouLi-na.2008.ComparisonofphysiologicalcharacteristicebetweentheleaveswithdifferentcoloursofCotinuscoggygria‘RoyalPurple’.JournalofNorthwestForestryUniversity,23(4):42～44.
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The 12. Wang Qiu months, Yu Jianping, Yang Wenkun. Masson Pine Bark procyanidins extraction and purification process is studied. the biological journal .2009 of mountain farming, 28 (5): 436 ~ 440.
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Claims (7)
1. from green pine needle, extract a method for haematochrome, it is characterized in that,
(1) take middle age or the biennial above green pine needle of maturity age pine tree, naturally dry after cleaning; Then stand-by after dry and soft for green pin being cut into segment;
(2) dry and soft for green pin and 1% methanol hydrochloride solution or 1% ethanol solution hydrochloride are added in leaching vessel, lixiviate 16-18 hour under indoor nature temperature, and pour out vat liquor when pine needle surface has been adsorbed a large amount of haematochrome and become red-brown;
(3) add the red pigments that 1% methanol hydrochloride solution or 1% ethanol solution hydrochloride wash-out are adsorbed on pine needle surface again, continue lixiviate 70-100 hour, pour out reddish-brown vat liquor stand-by; Add 1% methanol hydrochloride solution again or 1% ethanol solution hydrochloride continues lixiviate 70-100 hour among leaching vessel; Stand-by by mixing after above-mentioned twice vat liquor filtration residue or centrifugal removing impurity;
(4) reddish-brown extracted toward step (3) is extracted in stoste and is added NaOH, and adjustment solution ph, to 12-14, changes into after purple Precipitation until red pigments completely, and the red-purple powder obtained after centrifugal, drying, is pine needle haematochrome raw product.
2. a kind of method extracting haematochrome from green pine needle as claimed in claim 1, it is characterized in that, 1% methanol hydrochloride solution added for the 1st, 2,3 time or the mass ratio of 1% ethanol solution hydrochloride and the dry and soft pin of green are 12-20:12-20:12-20:1.
3. a kind of method extracting haematochrome from green pine needle as claimed in claim 2, is characterized in that, the mass ratio of described 1% methanol hydrochloride solution that adds for 1st, 2,3 time or 1% ethanol solution hydrochloride and the dry and soft pin of green is 16:16:16:1.
4. a kind of method extracting haematochrome from green pine needle as claimed in claim 1, is characterized in that, add the 1M sodium hydroxide that reddish-brown extracts stoste volume 1/13 in described step (4), adjust ph is 13.
5. a kind of method extracting haematochrome from green pine needle as claimed in claim 1, is characterized in that, centrifugal in described step (4) be 8000 revs/min centrifugal 10 minutes.
6. a kind of method extracting haematochrome from green pine needle as claimed in claim 1, is characterized in that, application water distilling apparatus reclaims methyl alcohol in vat liquor or ethanol.
7. a kind of method extracting haematochrome from green pine needle as claimed in claim 1, is characterized in that,
(1) take the biennial above green pine needle of maturity age pine tree, clean surperficial floating dust; Dry under Indoor Natural envrionment conditions; Then stand-by after being cut into the long segment of 1mm;
(2) by 1% methanol hydrochloride solution of dry and soft for green pin and its quality 16 times among leaching vessel, lixiviate 16-18 hour under indoor nature temperature, and when pine needle surface has been adsorbed a large amount of haematochrome and become red-brown, pour out vat liquor;
(3) add isopyknic 1% methanol hydrochloride solution is adsorbed on pine needle surface red pigments for wash-out again, continue lixiviate 75 hours, pour out reddish-brown vat liquor stand-by; Add isopyknic 1% hydrochloric acid methanol again and in leaching vessel, continue lixiviate 75 hours, mix after above-mentioned twice vat liquor filtration residue;
(4) ratio of 13:1 adds 1MNaOH in reddish-brown extraction stoste by volume, adjustment solution ph to 13, change into after purple Precipitation centrifugal 10 minutes with 8000 revs/min completely until red pigments after half an hour, outwell supernatant liquor, dried red-purple powder is pine needle haematochrome raw product;
(5) methyl alcohol in water distilling apparatus recovery vat liquor is applied.
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| CN1357382A (en) * | 2001-12-29 | 2002-07-10 | 南京大学 | Separating and purifying production process of proanthocyanidin oligomer from haw and its use |
| CN1436777A (en) * | 2003-03-07 | 2003-08-20 | 桂林莱茵生物制品有限公司 | Separation and extraction process of oligomer proanthocyanidin from pine bark |
| CN102796070A (en) * | 2012-08-29 | 2012-11-28 | 西南林业大学 | Preparation method of oligomeric proanthocyanidins |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1357382A (en) * | 2001-12-29 | 2002-07-10 | 南京大学 | Separating and purifying production process of proanthocyanidin oligomer from haw and its use |
| CN1436777A (en) * | 2003-03-07 | 2003-08-20 | 桂林莱茵生物制品有限公司 | Separation and extraction process of oligomer proanthocyanidin from pine bark |
| CN102796070A (en) * | 2012-08-29 | 2012-11-28 | 西南林业大学 | Preparation method of oligomeric proanthocyanidins |
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