CN104177863A - Method for extracting red pigment from green pin needles - Google Patents
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Abstract
The invention discloses a method for extracting a red pigment from green pin needles. The method comprises the following steps: extracting green pin needles with 1% hydrochloric acid methanol solution or 1% hydrochloric acid ethanol solution to obtain red-brown extract liquid, then precipitating by adding alkali, and then performing centrifugation and drying to obtain purplish-red powder which is the crude red pigment of pin needles. Experiments prove that the red pigment extracted from pin needles according to the method is a mixture of high-polymeric procyanidine and anthocyanidin as well as derivatives thereof; the invention proves that red procyanidine and anthocyanidin are produced during extraction, thereby greatly improving the yield of the red pigment of pin needles, and simultaneously large-scale production of the red pigment of pin needles provides a feasible choice for improving the color of pin needle tea and improving the quality of pin needle tea; and the method is simple, practical and low in cost, and is suitable for large-scale industrial production.
Description
Technical field
The present invention relates to a kind of method for extracting pigment, relate in particular to a kind of method of extracting haematochrome from green pine needle.
Background technology
Among plant organ especially petal, pericarp, tender leaf and fall foliage, extensively exist pigment miscellaneous, as cyanidin(e) (Chalker-Scott, 2002; Field et al., 2001; Gould et al., 1995; Zhang and Wang, 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) that once had thearubigins.Pine needle tea is as the existing merchandise sales of a kind of special health promoting beverage, but soup colour cast is light.The pine needle of green in evergreen needle, the especially season of growth of pine tree, 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 extraction (Wang Qiuyue etc., 2009) from the bark of pine tree mostly.For pine needle, pine tree bark resource quantity is less, especially from standing tree, strips off the skin comparatively inconvenient.Although there is the report (Huang Qiliang, 2012) that extracts pycnogenols from pine needle, the technique of directly extracting haematochrome from fresh green pine needle has no report.
The present inventor finds that colourless pycnogenols oxypolymerization forms red polymerization pycnogenols and cyanidin(e) (Cyanidin-3-O-glucoside etc.) in the process of using hydrochloric acid methanol (or acidic alcohol) lixiviate pine needle, thereby constantly has the mixture of haematochrome to be leached out.The method of at present conventional extraction pycnogenols is extracted mostly from the fruits such as grape, and output is subject to the impact in season, and the biennial bearing that produced by fruit affects.For other organ, pine needle stock number is larger, and season of growth appropriateness collection pine needle is little to the growth of pine tree and Survival Effects, and this creates conditions for producing in a large number pine needle haematochrome.
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 of 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 obtaining after centrifugal, dry, is pine needle haematochrome raw product.
Specifically comprise the following steps:
(1) take the biennial above green pine needle of middle age or maturity age pine tree, after cleaning, naturally dry; Then the dry and soft pin of green is cut into after segment stand-by;
(2) the dry and soft pin of green and 1% methanol hydrochloride solution are added in lixiviate container, lixiviate 16-18 hour at Indoor Natural temperature, and vat liquor (abandoning) is poured out on pine needle surface when having adsorbed a large amount of haematochrome and having become red-brown;
(3) add again 1% methanol hydrochloride solution wash-out to be adsorbed on the red pigments at the positions such as pine needle surface, constantly stir to improve extraction efficiency, continue lixiviate 70-100 hour, pour out reddish-brown vat liquor stand-by; Add again 1% methanol hydrochloride solution among lixiviate container, to continue lixiviate 70-100 hour; By above-mentioned twice vat liquor filtration residue or centrifugal remove mix after impurity stand-by;
(4) reddish-brown of extracting toward step (3) is extracted in stoste and is added NaOH, adjusts pH to 12-14, and after red pigments changes into purple Precipitation completely, the red-purple powder obtaining after centrifugal, dry, is pine needle haematochrome raw product.
In said extracted method, divide and add 1% methanol hydrochloride solution three times, preferably, 1% methanol hydrochloride solution that the 1st, 2,3 times add and the mass ratio of green dry and soft pin 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 hydrochloric acid that the concentration of 2.77ml is 36.5% adds methanol constant volume to 100ml.
In above-mentioned steps (4), preferably add reddish-brown to extract the 1M sodium hydroxide of stoste volume 1/13, regulating pH value is 13.
Centrifugal in above-mentioned steps (4), be preferably 8000 revs/min centrifugal 10 minutes.
In said extracted method, apply 1% acidic alcohol and substitute 1% hydrochloric acid methanol and can obtain pine needle haematochrome equally, and harmless with extraction using alcohol, but haematochrome extracted amount difference slightly.
In said extracted method, can apply water distilling apparatus and reclaim the discarded methyl alcohol of said process.
Through evidence, 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, is bluish voilet in alkaline environment, under sour environment, is red-brown.
Application: add in pine needle tea, increase pine needle liquor color, can also be used as food or drug additive.
The present invention proves by experimental study, and this technique can extract red pigments from green pine needle, and is accompanied by the increase of drying treatment degree and improves the extracted amount of haematochrome.Present method is utilized the principle of the cuticular macromole fatty acid ester absorption of pine needle red pigments, by extraction reasonable in design and elution process, has played 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 can bring up to 10%-18%.
Because pine needle output is large, evergreen all the year round, from pine needle, extract haematochrome and be not substantially subject to stock number and seasonal impact.The present invention proves that red high polymerization pycnogenols and cyanidin(e) produce in leaching process, and this significantly improves the output of pine needle haematochrome, even surpasses bark.A large amount of productions of pine needle haematochrome for increasing pine needle liquor color, improve pine needle tea quality a kind of feasible selection be provided.Present method is simple and practical, with low cost, is suitable for industrial a large amount of production.
Accompanying drawing explanation
Fig. 1 is that while using methanol hydrochloride solution lixiviate pine needle, haematochrome produces the microscopic examination at position and the variation of vat liquor color; A. hydrochloric acid methanol lixiviate pine needle horny layer of epidermis variation after 24 hours, finds that there is anthocyanin and forms; 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 after 24 hours pine needle horny layer of epidermis and endodermis change, find that pine needle horny layer of epidermis and endodermis are without the significantly formation of anthocyanin; 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 variation 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 relatively; Wherein CK be normal pine needle in contrast, Rw is the needle of rehydration again after dehydration;
Fig. 5 is the fresh needle of black pine, dry needle, needle, the contrast of the anthocyanin extracted amount of needle, Pollen pini thunbergii bark and Japanese red pine skin for many years then;
Fig. 6 is pine needle and bark extracting solution and sedimentary RGB image analysis; A. the G/R value that pine needle pigment powder redissolution thing (L-n), bark pigment powder redissolve thing (P-n), pine needle extract (L-o), bark extracting solution (P-o), pine needle throw out (L-d) and bark throw out (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 that the embodiment of the present invention 4 is extracted the process flow sheet of red pigments from green pine needle.
Embodiment
The impact on extraction effect such as the water content of 1 extraction time of embodiment and extracting solution
The present invention adopts 1% hydrochloric acid methanol to extract black pine (Pinus thunbergii Parl.) pine needle haematochrome.Research is found, during with hydrochloric acid methanol lixiviate black pine pine needle, starts to take green pigment as main in vat liquor, does not almost have haematochrome to extract (in 5 hours) (Fig. 1 d).Be accompanied by the prolongation of extraction time, in methanol hydrochloride solution, also gradually by blue green, change into yellow-green colour.On pine needle surface, (Fig. 1 a) He in endodermis cell (Fig. 1 b) engenders red pigments, and the haematochrome at this moment producing is attracted to above cuticular macromole fatty acid ester mostly.With the continuation of extraction time, extend, be accompanied by the chlorophyll composition that extracts decomposition (Feng et al., the 2009) extracting solution under illumination and become red-brown (Fig. 1 e) through red-purple.In normal room temperature environment, completing extraction needed between 300 to 400 hours.This leaching process is influenced by environmental temperature, the progress of heating and can shorten extraction time and accelerating to extract.In order to save extraction cost, the present invention only extracts under natural room temperature.While by contrast, using 50%:50% hydrochloric acid methanol-water mixed liquid body (Gong etc. 2004) lixiviate, without obvious haematochrome, form (Fig. 1 c) and almost do not have haematochrome to be extracted.
The absorbancy of using visible spectrophotometer to measure 100% hydrochloric acid methanol extracting solution of pine needle at 525nm wave band finds, the corresponding OD value of increase that is accompanied by extraction time improves gradually, until within more than 300 hour, just settle out gradually (Fig. 2-100).While extracting identical pine needle in the miscible system of acidic methanol-water 90% (10% water+90% hydrochloric acid methanol) (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.While extracting identical pine needle in the acidic methanol-water immiscible liquid 50% (50% water+50% hydrochloric acid methanol) (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.
Further dwindle between the miscible liquid gradient to 85% of methanol-water and 100% that (Fig. 3 a),, to (Fig. 3 b) between 95% and 100%, even between to 99% to 100%, the trend reducing with the increase red pigments growing amount of water content still exists.Therefore, with hydrochloric acid methanol, extract the impact that pine needle haematochrome is subject to the water content of extracting solution.And adopting hydrochloric acid methanol to extract pine needle haematochrome need to have lasting an immersion to make pine needle oxypolymerization and change the process that colourless pycnogenols becomes haematochrome.
Embodiment 2 impacts of pine needle water ratio on extraction effect
Pine needle water ratio is shown in Fig. 4 and Fig. 5 to the impact of extraction effect, the data of Fig. 4 show, the needle haematochrome extracted amount of processed obviously increases, and (Fig. 4 a) between the haematochrome absorbance of pine needle water ratio and extracting solution, obvious linear dependence relation.The pine needle of drying treatment after rehydration is processed again, is compared with the not withering pine needle that contrasts, and haematochrome extracting solution does not have the difference (Fig. 4 b) on statistical significance.
This tests explanation, and the process of extracting pine needle haematochrome with hydrochloric acid methanol is a process for oxypolymerization gradually, and drying treatment pine needle is conducive to improve the extracted amount of pine needle haematochrome.In addition, except drying and dehydrating can improve pine needle haematochrome extracted amount, perennial pine needle ratio is the haematochrome quantum of output high (Fig. 5) of newborn pine needle then.The extracted amount of pine needle haematochrome is even higher than bark (Fig. 5), especially dried needle.The red pigments amount of extracting from dry green pine needle is even higher than withered pine needle russet.
Embodiment 3 pine needle haematochrome composition analyses
Research shows, the red solution color after alkaline sedimentation that continues the green pine needle generation of lixiviate in acidic methanol solution becomes bluish voilet (Fig. 6 a-Ld, Fig. 6 b-Ld), although also having, the BS of bark extracting solution becomes lilac trend, its degree is than pine needle much lower (Fig. 6 a-Pd, Fig. 6 b-Pd).This points out the formation that has 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 present invention is a process for oxypolymerization gradually by the process that hydrochloric acid methanol extracts pine needle haematochrome, and colourless oligomeric procyanidolics is converted into the high polymerization pycnogenols (Huang Qiliang, 2012) of reddish-brown through oxypolymerization.
In order further to prove the existence of high polymerization pycnogenols and cyanidin(e), carry out following test: 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), process high performance liquid chromatography and mass spectrum are used in conjunction to analyze and show that in this extracting solution, existing high polymerization pycnogenols also has cyanidin(e).Its wave spectrogram looks like to see Fig. 7, and its assay result is as table 1.Therefore, prove that the red pigments forming is the mixture of high polymerization pycnogenols and cyanidin(e) and derivative thereof in the lasting leaching process of methanol hydrochloride solution.Apply suitable separation means and can produce the pine needle haematochrome with certain activity.
Cyanidin-3-O-glucoside and catechin content in table 1 vat liquor
| Component numbering | 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; Under Indoor Natural environment (temperature 25-35 ℃, relative humidity 50-70%) condition, dry; Then be cut into after the long segment of 1mm stand-by;
(2) by 1% methanol hydrochloride solution of the dry and soft pin of green and 16 times of quality (in the dry and soft pin of green) among lixiviate container, lixiviate 16-18 hour at Indoor Natural temperature, and when pine needle surface has been adsorbed a large amount of haematochrome and become red-brown, pour out yellow-green colour or brown vat liquor; The compound method of 1% methanol hydrochloride solution is: the hydrochloric acid that the concentration of 2.77ml is 36.5% adds methanol constant volume to 100ml;
(3) add again isopyknic 1% methanol hydrochloride solution for wash-out, to be adsorbed on the red pigments at the positions such as pine needle surface, constantly stir to improve extraction efficiency, continue lixiviate 75 hours, pour out reddish-brown vat liquor stand-by; Add again isopyknic 1% hydrochloric acid methanol in lixiviate container, to continue lixiviate 75 hours, will after above-mentioned twice vat liquor filtration residue, mix;
(4) ratio of 13:1 is extracted in stoste and is added 1M NaOH toward reddish-brown by volume, adjust pH to 13, centrifugal 10 minutes with 8000 revs/min after red pigments changes into purple Precipitation completely after half an hour, outwell supernatant liquor, dried red-purple powder is pine needle haematochrome raw product; Extraction yield is 12-18%;
(5) application water distilling apparatus reclaims 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; Under Indoor Natural environment (temperature 25-35 ℃, relative humidity 50-70%) condition, dry; Then be cut into after the long segment of 1mm stand-by; The compound method of 1% ethanol solution hydrochloride is: the hydrochloric acid that the concentration of 2.77ml is 36.5% adds ethanol to be settled to 100ml;
(2) by 1% ethanol solution hydrochloride of the dry and soft pin of green and 18 times of quality (in the dry and soft pin of green) among lixiviate container, lixiviate 16-18 hour at Indoor Natural temperature, and when pine needle surface has been adsorbed a large amount of haematochrome and become red-brown, pour out yellow-green colour or brown vat liquor;
(3) add again isopyknic 1% ethanol solution hydrochloride for wash-out, to be adsorbed on the red pigments at the positions such as pine needle surface, constantly stir to improve extraction efficiency, continue lixiviate 80 hours, pour out reddish-brown vat liquor stand-by; Add again isopyknic 1% acidic alcohol in lixiviate container, to continue lixiviate 80 hours, will after above-mentioned twice vat liquor filtration residue, mix;
(4) ratio of 13:1 is extracted in stoste and is added 1M NaOH toward reddish-brown by volume, adjust pH to 13, centrifugal 10 minutes with 8000 revs/min after red pigments changes into purple Precipitation completely after half an hour, outwell supernatant liquor, dried red-purple powder is pine needle haematochrome raw product; Its extraction yield is 10-15%;
(5) application water distilling apparatus reclaims the discarded ethanol of said process.
Reference
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Claims (9)
1. a method of extracting haematochrome from green pine needle, it is characterized in that, adopt the green pine needle of 1% methanol hydrochloride solution or 1% ethanol solution hydrochloride lixiviate to obtain reddish-brown vat liquor, then add alkali precipitation, the red-purple powder obtaining after centrifugal, dry, is pine needle haematochrome raw product.
2. a kind of method of extracting haematochrome from green pine needle as claimed in claim 1, is characterized in that,
(1) take the biennial above green pine needle of middle age or maturity age pine tree, after cleaning, naturally dry; Then the dry and soft pin of green is cut into after segment stand-by;
(2) the dry and soft pin of green and 1% methanol hydrochloride solution or 1% ethanol solution hydrochloride are added in lixiviate container, lixiviate 16-18 hour at Indoor Natural temperature, and vat liquor is poured out on pine needle surface when having adsorbed a large amount of haematochrome and having become red-brown;
(3) add again 1% methanol hydrochloride solution or 1% ethanol solution hydrochloride wash-out to be adsorbed on the red pigments on pine needle surface, continue lixiviate 70-100 hour, pour out reddish-brown vat liquor stand-by; Add again 1% methanol hydrochloride solution or 1% ethanol solution hydrochloride among lixiviate container, to continue lixiviate 70-100 hour; By above-mentioned twice vat liquor filtration residue or centrifugal remove mix after impurity stand-by;
(4) reddish-brown of extracting toward step (3) is extracted in stoste and is added NaOH, adjusts pH to 12-14, and after red pigments changes into purple Precipitation completely, the red-purple powder obtaining after centrifugal, dry, is pine needle haematochrome raw product.
3. a kind of method of extracting haematochrome from green pine needle as claimed in claim 2, is characterized in that, 1% methanol hydrochloride solution that the 1st, 2,3 times add or the mass ratio of 1% ethanol solution hydrochloride and green dry and soft pin are 12-20:12-20:12-20:1.
4. a kind of method of extracting haematochrome from green pine needle as claimed in claim 3, is characterized in that, the mass ratio of described 1% methanol hydrochloride solution adding for the 1st, 2,3 times or 1% ethanol solution hydrochloride and green dry and soft pin is 16:16:16:1.
5. a kind of method of extracting haematochrome from green pine needle as claimed in claim 2, is characterized in that, adds reddish-brown to extract the 1M sodium hydroxide of stoste volume 1/13 in described step (4), and regulating pH value is 13.
6. a kind of method of extracting haematochrome from green pine needle as claimed in claim 2, is characterized in that, centrifugal in described step (4) be 8000 revs/min centrifugal 10 minutes.
7. a kind of method of extracting haematochrome from green pine needle as claimed in claim 2, is characterized in that, application water distilling apparatus reclaims methyl alcohol or the ethanol in vat liquor.
8. a kind of method of extracting haematochrome from green pine needle as claimed in claim 2, is characterized in that,
(1) take the biennial above green pine needle of maturity age pine tree, clean surperficial floating dust; Under Indoor Natural envrionment conditions, dry; Then be cut into after the long segment of 1mm stand-by;
(2) by 1% methanol hydrochloride solution of 16 times of the dry and soft pin of green and its quality among lixiviate container, lixiviate 16-18 hour at Indoor Natural temperature, and pine needle surface has been adsorbed a large amount of haematochrome and while becoming red-brown, poured out vat liquor;
(3) add again isopyknic 1% methanol hydrochloride solution for wash-out, to be adsorbed on the red pigments on pine needle surface, continue lixiviate 75 hours, pour out reddish-brown vat liquor stand-by; Add again isopyknic 1% hydrochloric acid methanol in lixiviate container, to continue lixiviate 75 hours, will after above-mentioned twice vat liquor filtration residue, mix;
(4) ratio of 13:1 is extracted in stoste and is added 1M NaOH toward reddish-brown by volume, adjust pH to 13, centrifugal 10 minutes with 8000 revs/min after red pigments changes into purple Precipitation completely after half an hour, outwell supernatant liquor, dried red-purple powder is pine needle haematochrome raw product;
(5) application water distilling apparatus reclaims the methyl alcohol in vat liquor.
9. the pine needle haematochrome that in claim 1-8, the method described in any one is extracted, is characterized in that, its main component is high polymerization pycnogenols and cyanidin(e).
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| CN109646993A (en) * | 2019-01-30 | 2019-04-19 | 山东省林业科学研究院 | A kind of method and apparatus for the red degradation product extracting plant chlorophyll |
| CN114145142A (en) * | 2021-11-19 | 2022-03-08 | 重庆市林业科学研究院 | Cluster bamboo industrial cuttage method |
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| CN107087698A (en) * | 2017-05-16 | 2017-08-25 | 云南农业大学 | A kind of method for producing purple beautiful instant tea |
| CN109646993A (en) * | 2019-01-30 | 2019-04-19 | 山东省林业科学研究院 | A kind of method and apparatus for the red degradation product extracting plant chlorophyll |
| CN109646993B (en) * | 2019-01-30 | 2020-12-22 | 山东省林业科学研究院 | Method and device for extracting red degradation product of plant chlorophyll |
| CN114145142A (en) * | 2021-11-19 | 2022-03-08 | 重庆市林业科学研究院 | Cluster bamboo industrial cuttage method |
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