CN103319912B - Hickory nut shell brown pigment and its preparation method - Google Patents
Hickory nut shell brown pigment and its preparation method Download PDFInfo
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- CN103319912B CN103319912B CN201310302398.XA CN201310302398A CN103319912B CN 103319912 B CN103319912 B CN 103319912B CN 201310302398 A CN201310302398 A CN 201310302398A CN 103319912 B CN103319912 B CN 103319912B
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Abstract
An extraction method of a high-performance and high-stability Northeast hickory nut shell brown pigment relates to a natural pigment processing technology. According to the invention, compound enzyme-supersonic wave-supercritical are creatively and effectively combined in synergism. Thus, residues require no secondary digestion or extraction but only require extraction once so as to effectively avoid the influence of secondary extraction on pigment activity. With the cooperation of compound enzyme, extraction rate is greatly raised, and the influence of fat on the pigment is avoided. The whole course is carried out at a low and mild temperature, thus guaranteeing the pigment activity and activity stability and achieving an unexpected technical effect. The preparation method provided by the invention has advantages of simple technology, short period and no complex equipment, is easy to operate, is adopted to obviously raise product performance, and is suitable for industrial production.
Description
Technical field
The invention provides a kind of purity good, the brown pigmentation that performance is high, stability is high, relates to natural pigment processing technology, belongs to food chemistry processing technique field.
Background technology
Edible natural pigment refers to the food dye obtaining from natural resource, has plenty of from the edibility extracting section of long-term edible organism; Have plenty of and extract from the root of medicine food dual purpose plant, stem, leaf, fruit; Have plenty of from the shell of organism or pericarp and extract.Can find out from the source of natural pigment, most of natural pigments are safe, and human body is almost had no adverse effects, and can be used as healthy food dye.
Heilongjiang Province's forest land resource is very luxuriant, and forest land area is 2427.6 ten thousand hectares, ranks first in the country, and accounts for 51.3% of the whole province's soil total area.Mountain local product is of a great variety, standing stock are large, and Semen Caryae Cathayensis is just one of wherein important nut.Along with the expansion year by year of walnut product amount of finish, the main byproduct nut-shell of walnut processing has also caused people's concern.Past nut-shell is dropped or is burned, and has caused the significant wastage of resource.After having occurred that in recent years nut-shell is processed as to gac, make fuel, improved the added value of nut-shell.The further investigation of nut-shell is found, in nut-shell, contain natural brown pigmentation, if this natural pigment can be extracted, and for food-processing, both avoided the waste of nut-shell resource, meet again the demand of people to healthy, safe natural pigment, embodied fully the value of nut-shell comprehensively.
Northeast Semen Caryae Cathayensis is due to unique region, other place of production of hardness ratio of pecan shell higher, draw world elite, contained pigment quality is high, and in prior art, conventionally all directly adopt extraction or hyperacoustic independent method to extract, exist extraction time long, obtain pigment product poor quality, the active shortcoming such as low.At present, the research of pecan shell brown pigmentation extraction aspect, domestic northeast, focus on the pigment crude product of high yield, biological activity, purity and the extraction efficiency of product are ignored, and be all secondary lixiviate conventionally, time is long, increases production cost and process complexity, and quality is low cannot meet the demand to high-end pigment product on market.Do not have the prozyme of zymin, especially specific proportioning to be used in the pigment extraction of northeast pecan shell yet.Also there is no at present a kind of effective ways that northeast Semen Caryae Cathayensis pigment extracts that are exclusively used in.Therefore, for the special raw material resources of high-quality, provide a kind of effectively extracting method, just become one of current industry problem demanding prompt solution.
Also not yet have at present prozyme-ultrasonic wave-overcritical associating used to the report that pecan shell pigment extracts northeastward.
Summary of the invention
Object of the present invention: provide that one has that technique is simple, easy handling, cycle are short, without complex apparatus, obviously enhance product performance, be applicable to the extracting method of the pecan shell brown pigmentation of the advantages such as suitability for industrialized production, effectively utilize nut-shell resource.
Technical scheme of the present invention: the extracting method of a kind of high-performance, high stability pecan shell brown pigmentation, is characterized in that preparing according to following steps:
(1), by pecan shell decon, clear water rinses, and at 35 DEG C of-38 DEG C of temperature, dries, and is ground into 40-80 object powder for subsequent use;
(2) according to 1: 30-1: powder is added ethanol-citric acid system by 33 solid-liquid ratio (w/v), fully soak wetting, in extracting solution, add again cellulase, hemicellulase, polygalacturonase and lipase, the addition of enzyme is the 0.003%-0.008% of walnut powder quality, and its cellulase, hemicellulase, polygalacturonase and lipase ratio are 3: 2: 1: 1; Wherein, ethanol-citric acid system is: using citric acid as solute, the aqueous ethanolic solution taking 50% is solvent, and being mixed with concentration by quality volume percent is citric acid-ethanolic soln of 0.1%;
(3) ultrasonication: the mixture in step (2) is carried out to ultrasonication, and ultrasonic power is 300w-350w, ultrasonic temperature is 35 DEG C-38 DEG C, extracts 40min-50min;
(4) supercritical extraction: step (3) is carried out to supercritical extraction again through the mixture of ultrasonication, and pressure is 15MPa-20MPa, and temperature is 35 DEG C-38 DEG C, and the time is 0.5h-1h; Obtain crude extract; Preferably supercritical CO
2extraction, CO
2flow 26L/h.
(5) crude extract filters, and filtrate centrifugation under 5000r/min, 5min condition, obtains centrifugate, centrifugate is carried out to cryogenic vacuum and concentrate, pressure is 0.085MPa-0.090MPa, and temperature is 35 DEG C-38 DEG C, the 1/2-1/3 that is concentrated into original volume, obtains concentrated solution;
(6) absorption: by polar macroporous NKA-9 on concentrated solution resin column, loading flow velocity is 1mL/min-3mL/min, extremely saturated through macroporous resin adsorption brown pigments;
(7) wash-out: wash away the debris and the weak water-soluble impurity of adsorptive power that are not adsorbed with the water (V/V) that is no less than 2 times of column volumes, wash away middle polarity impurity with the aqueous ethanolic solution (V/V) of the 15-30% that is no less than 3 times of column volumes again, finally use citric acid-ethanol elution brown pigmentation of 0.1%, elution flow rate is 0.5mL/min-2.0mL/min
(8) vacuum concentration: preferably elutriant is under 0.085MPa-0.090MPa, 35 DEG C of-38 DEG C of conditions, and vacuum concentration becomes brown pigments concentrated solution;
(9) lyophilize: preferably by concentrated solution under-50 DEG C～38 DEG C conditions, lyophilize 25h-32h, obtains brown pigments powder.Wherein, an another technical scheme is that the step of (6), (7), (8) is omitted.Preferably supercritical extraction adopts supercritical co.Preferably CO
2flow 26L/h.
Beneficial effect of the present invention:
(1) on the basis of early-stage Study, creatively prozyme-ultrasonic wave of contriver-overcritical is carried out effective combination, synergy mutually, make residue not need secondary lixiviate or extraction, ultrasonic wave is also only once ultrasonic, only need lixiviate once, effectively avoid second extraction on the active impact producing of pigment; Wherein, the effect of prozyme: cellulase and hemicellulase are hydrolyzed the Mierocrystalline cellulose in shell in the mode of going forward one by one, nut-shell also belongs to vegetable cell, contriver innovates trial polygalacturonase, finds that unexpectedly in cellulase combining pectin enzyme better changes the permeability of cell walls, makes histocyte inclusion fully contact with solvent, make the quick solution transfer of effective constituent, thereby change the permeability of cell walls, accelerate the release of pigment, thereby improve extraction yield.In addition use lipase, the effectively use of petroleum replacing ether, thoroughly removes from inside to outside and reduces fat, and eliminates the impact of sherwood oil on pigment quality in whole process.
Contriver finds unexpectedly, when in conjunction with ultrasonic wave and supercritical extraction time, do not abandon the use of enzyme, the interpolation of cellulase, hemicellulase, polygalacturonase and lipase that mass ratio is 0.003-0.008%, more be conducive to the stripping of pigment, greatly saved the usage quantity of enzyme; Cellulase, hemicellulase, polygalacturonase and lipase ratio 3: 2: 1: 1 has novelty, does not use four kinds of enzymes and in described ratio, pecan shell pigment is extracted in prior art.
Ultrasonic wave is a kind of elastic mechanical ripple, swirling effect, cavitation effect and the heat effect of utilizing Ultrasonic Radiation pressure to produce changes material weave construction, state, function or accelerates the process of these changes, can make generation circulation in cell peripheral and cell, thereby improve the permeability of cell walls and cytolemma, played the effect of strengthening extraction process, be conducive to the extraction of effective constituent in cell, shorten extraction time, extraction rate is fast, economizes solvent, save energy.Supercritical CO
2the features such as abstraction technique has no solvent residue, extraction yield is high, product purity is high, can prevent the oxidation of heat-sensitive substance composition and volatilization, the loss of pigment natural radioactivity is little and pollution-free, noresidue, meet environmental requirement, product quality compared with advantages of higher.Other suitable supercutical fluids are also passable.
Prozyme-ultrasonic wave-overcritical is carried out effective combination, and synergy, has produced and be greater than prozyme+ultrasonic wave+postcritical technique effect mutually.Overcritical in conjunction with the short period of time, greatly reduces cost, enhances product performance.
(2) simultaneously, trier finds unexpectedly, and in the technique before lyophilize, 35 DEG C of-38 DEG C of low temperature of whole process using, gentle temperature are carried out, and have ensured the activity of pigment, and active stability, have obtained the technique effect that contriver is difficult to expect.
(3) the each performance of product is all improved significantly, and the target product that the present invention obtains is the synergistic result of each processing parameter, has produced unforeseeable technique effect.
Product property evaluation method is as follows, (also can adopt other ordinary method of this area to evaluate): controlled trial adopt use separately solvent or ultrasonic method extract, also can be taking solvent and ultrasonic wave coupling as contrast.Also can be taking traditional method other method in contrast or prior art.
1, the extraction yield of nut-shell brown pigments: (yield) %=brown pigments powder (g)/nut-shell powder (g) × 100%.Yield of the present invention is at 9-10%, and in different controlled trial, extraction yield is up to 4-5%.
2, the spectral response curve of nut-shell brown pigments
The brown pigments solution of 50 μ g/ml is measured in 250nm-400nm wavelength region to its characteristic absorption spectrum with ultraviolet-visible pectrophotometer, taking distilled water as contrast.The aqueous solution of nut-shell pigment has maximum absorption band at 289nm place, therefore test and Selection 289nm is as the foundation of quantitative measurment.
3, the impact of potential of hydrogen on brown pigments
The pigment solution of 6 parts of 25ml50 μ g/ml is joined in the solution of the different pH value that 10ml NaOH or hydrochloric acid is made into, vibration, leave standstill after 2h, with pH test paper record that pH value of solution is respectively 2～3,5-6,7～8,9-10,11-12,13-14, measure its light absorption value.
The present invention, in pH7～8 absorbancy maximum, still has greatlyr in absorbancy when pH2～3,11-12, product resistance to acids and bases of the present invention is stronger.Light absorption value general trend is to increase with pH value, and light absorption value declines.
4, light stability
The pigment solution 10ml Continuous irradiation 25d under daylight that gets 1 part of 50 μ g/ml, measures its light absorption value every day, analyzes the impact of illumination on this brown pigments solution.
The present invention: along with the growth of sunshine duration, the light absorption value of brown pigments solution in the time of 289nm reduces gradually, after 25d color thin out but without precipitation generate.; And the color of control group is obviously thin out, and there is precipitation to generate.
5, thermostability
Get the pigment solution of 5 part of 50 μ g/ml, in the time of 20 DEG C, 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C, 70 DEG C, 80 DEG C, 90 DEG C, 100 DEG C, heat respectively 1h, measure light absorption value.The impact of analysis temperature on this brown pigments solution.
The better heat stability of the application below 93 DEG C, even can tolerate 100 DEG C of short period of time, and all becomes unstable when 80 DEG C of control groups.
6, the impact of Oxidizing and Reducing Agents on brown pigments
Get three parts of the brown pigments solution of 50 μ g/ml, add respectively 0%, 0.1%, 0.4%, 0.6%, 0.8% H
2o
2solution, places after 2h, measures its absorbancy.Separately get three parts of the brown pigments solution of 50 μ g/ml, add respectively 0%, 0.4%, 0.6%, 0.8% Na
2sO
3solution, places the light absorption value of measuring respectively pigment solution after 2h.
The present invention is along with the increase of Oxidizing and Reducing Agents concentration, and the absorbancy of nut-shell brown pigments slightly reduces, but changes not quite, illustrates that certain density Oxidizing and Reducing Agents is less on the impact of brown pigments, and anti-oxidant reducing power is stronger; And control group is along with the increase of Oxidizing and Reducing Agents concentration, larger on the absorbance impact of nut-shell brown pigments, a little less than illustrating that its anti-oxidant reducing power.
7, the impact of metal ion on brown pigments
The brown pigments solution of preparing 6 parts of 10ml50 μ g/ml, adds respectively Na
+, Fe
3+, Ca
2+, Mg
2+, Cu
2+, Al
3+10mg and 10ml distilled water, measure respectively its light absorption value.
Metal ion Na of the present invention
+, Fe
3+, Mg
2+, Ca
2+, Al
3+, Cu
2+dilute solution be more stable, these ions within the specific limits can stable existence; And control group is also more stable, but Cu
2+, Fe
3+have an impact to brown.
8. anti-oxidant activity
Adopt Tripotassium iron hexacyanide reduction method to measure the brown pigments that the present invention obtains, its anti-oxidant activity can reach the 25%-30% of Vc, and with control group or traditional method comparison, reducing power can improve 10%-10.6%.
This property of pigment is high, and stablizing can be in the stronger cola of the plain fastidious property of checking colors; Conventionally, in pigment application process, should avoid adding phenylformic acid, and nut-shell pigment of the present invention also there is certain resistance to the phenylformic acid that should not add.
Embodiment
Embodiment 1: the extracting method of a kind of high-performance, high stability pecan shell brown pigmentation, is characterized in that preparing according to following steps:
(1), by pecan shell decon, clear water rinses, and at 36 DEG C of temperature, dries, and is ground into 60 object powder for subsequent use;
(2) according to the solid-liquid ratio (w/v) of 1: 32, powder is added to ethanol-citric acid system, fully soak wetting, in extracting solution, add again cellulase, hemicellulase, polygalacturonase and lipase, the addition of enzyme is walnut powder quality 0.005%, and its cellulase, hemicellulase, polygalacturonase and lipase ratio are 3: 2: 1: 1; Wherein, ethanol-citric acid system is: using citric acid as solute, the aqueous ethanolic solution taking 50% is solvent, and being mixed with concentration by quality volume percent is citric acid-ethanolic soln of 0.1%;
(3) ultrasonication: the mixture in step (2) is carried out to ultrasonication, and ultrasonic power is 330w, and ultrasonic temperature is 36 DEG C, extracts 45min;
(4) supercritical extraction: step (3) is carried out to supercritical extraction again through the mixture of ultrasonication, and pressure is 18MPa, and temperature is 36 DEG C, and the time is 1h; Obtain crude extract; Preferably, supercritical CO
2flow 26L/h.
(5) crude extract filters, and filtrate centrifugation under 5000r/min, 5min condition, obtains centrifugate, centrifugate is carried out to cryogenic vacuum and concentrate, and pressure is 0.085MPa-0.090MPa, and temperature is 36 DEG C, is concentrated into the 1/2-1/3 of original volume, obtains concentrated solution;
(6) absorption: by polar macroporous NKA-9 on concentrated solution resin column, loading flow velocity is 1mL/min-3mL/min, extremely saturated through macroporous resin adsorption brown pigments;
(7) wash-out: wash away the debris and the weak water-soluble impurity of adsorptive power that are not adsorbed with the water (V/V) that is no less than 2 times of column volumes, wash away middle polarity impurity with the aqueous ethanolic solution (V/V) of the 15%-30% that is no less than 3 times of column volumes again, finally use citric acid-ethanol elution brown pigmentation of 0.1%, elution flow rate is 0.5mL/min-2.0mL/min;
(8) elutriant is under 0.085MPa-0.090MPa, 36 DEG C of conditions, and vacuum concentration becomes brown pigments concentrated solution;
(9) by concentrated solution under-50 DEG C of-38 DEG C of conditions, lyophilize 29h, obtains brown pigments powder.
Embodiment: 2: the extracting method of a kind of high-performance, high stability pecan shell brown pigmentation, is characterized in that preparing according to following steps:
(1), by pecan shell decon, clear water rinses, and at 36 DEG C of temperature, dries, and is ground into 60 object powder for subsequent use;
(2) according to the solid-liquid ratio (w/v) of 1: 32, powder is added to ethanol-citric acid system, fully soak wetting, in extracting solution, add again cellulase, hemicellulase, polygalacturonase and lipase, the addition of enzyme is walnut powder quality 0.005%, and its cellulase, hemicellulase, polygalacturonase and lipase ratio are 3: 2: 1: 1; Wherein, ethanol-citric acid system is: using citric acid as solute, the aqueous ethanolic solution taking 50% is solvent, and being mixed with concentration by quality volume percent is citric acid-ethanolic soln of 0.1%;
(3) ultrasonication: the mixture in step (2) is carried out to ultrasonication, and ultrasonic power is 330w, and ultrasonic temperature is 36 DEG C, extracts 45min;
(4) carbon dioxide upercritical fluid extraction: step (3) is carried out to supercritical extraction again through the mixture of ultrasonication, and pressure is 18MPa, and temperature is 36 DEG C, and the time is 1h; Obtain crude extract; Preferably CO
2flow 26L/h.
(5) crude extract filters, and filtrate centrifugation under 5000r/min, 5min condition, obtains centrifugate, centrifugate is carried out to cryogenic vacuum and concentrate, and pressure is 0.085MPa-0.090MPa, and temperature is 36 DEG C, is concentrated into the 1/2-1/3 of original volume, obtains concentrated solution; (6) absorption: by polar macroporous NKA-9 on concentrated solution resin column, loading flow velocity is 1mL/min-3mL/min, extremely saturated through macroporous resin adsorption brown pigments;
(7) wash-out: wash away the debris and the weak water-soluble impurity of adsorptive power that are not adsorbed with the water (V/V) that is no less than 2 times of column volumes, wash away middle polarity impurity with the aqueous ethanolic solution (V/V) of the 15-30% that is no less than 3 times of column volumes again, finally use citric acid-ethanol elution brown pigmentation of 0.1%, elution flow rate is 0.5mL/min-2.0mL/min;
(8) elutriant is under 0.085MPa-0.090MPa, 36 DEG C of conditions, and vacuum concentration becomes brown pigments concentrated solution;
(9) by concentrated solution under-50 DEG C of-38 DEG C of conditions, lyophilize 29h, obtains brown pigments powder.
Claims (1)
1. an extracting method for pecan shell brown pigmentation, is characterized in that preparing according to following steps:
(1), by pecan shell decon, clear water rinses, and at 35-38 DEG C of temperature, dries, and is ground into 40-80 object powder for subsequent use; Semen Caryae Cathayensis is the Wild hickory on Changbai Mountain, northeast;
(2) according to 1: 30-1: 33 solid-liquid ratio, be w/v, powder is added to ethanol-citric acid system, fully soak wetting, add again cellulase, hemicellulase, polygalacturonase and lipase, the addition of enzyme is the 0.003-0.008% of walnut shell flour quality, and its cellulase, hemicellulase, polygalacturonase and lipase ratio are 3: 2: 1: 1; Wherein, ethanol-citric acid system is: using citric acid as solute, the aqueous ethanolic solution taking 50% is solvent, and being mixed with concentration by quality volume percent is citric acid-ethanolic soln of 0.1%; In the whole system of step (2), pH adjusts or remains on 3-6;
(3) ultrasonication: the mixture of step (2) is carried out to ultrasonication, and ultrasonic power is 300w-350w, ultrasonic temperature is 35 DEG C-38 DEG C, extracts 40min-50min;
(4) supercritical extraction: step (3) is carried out to supercritical extraction again through the mixture of ultrasonication, and pressure is 15-20MPa, and temperature is 35 DEG C-38 DEG C, and the time is 0.5-1h; Obtain crude extract; Overcritical employing CO 2 supercritical, CO
2flow 26L/h;
(5) crude extract filters, and filtrate centrifugation under 5000r/min, 5min condition, obtains centrifugate, centrifugate is carried out to cryogenic vacuum and concentrate, pressure is 0.085-0.090MPa, and temperature is 35-38 DEG C, the 1/2-1/3 that is concentrated into original volume, obtains concentrated solution;
(6) absorption: by polar macroporous NKA-9 on concentrated solution resin column, loading flow velocity is 1-3mL/min, extremely saturated through macroporous resin adsorption brown pigments;
(7) wash-out: with the water that is no less than 2 times of column volumes, V/V, wash away the debris and the weak water-soluble impurity of adsorptive power that are not adsorbed, use again the aqueous ethanolic solution of the 15-30% that is no less than 3 times of column volumes, V/V, wash away middle polarity impurity, finally use citric acid-ethanol elution brown pigmentation of 0.1%, elution flow rate is 0.5-2.0mL/min;
(8) elutriant is under 0.085-0.090MPa, 35-38 DEG C condition, and vacuum concentration becomes brown pigments concentrated solution;
(9) by concentrated solution under-50 DEG C～38 DEG C conditions, lyophilize 25h-32h, obtains brown pigments powder.
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| CN104910643A (en) * | 2015-06-08 | 2015-09-16 | 昆明理工大学 | Method for extracting walnut-shell brown pigments |
| CN105064076B (en) * | 2015-09-08 | 2017-12-26 | 绍兴圣苗针纺有限公司 | A kind of cotton fabric dyeing process method using walnut shell pigment |
| CN106118129A (en) * | 2016-07-13 | 2016-11-16 | 阜南县大喜柳编工艺品有限公司 | A kind of bronze-colored stain of knitting |
| CN113801493A (en) * | 2021-10-14 | 2021-12-17 | 锦柯草木染(上海)纺织科技有限公司 | Method for extracting natural dye from outer skin of pecan |
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