CN105038306A - Method for extracting watermelon red coloring matter with assistance of floatation impurity removal - Google Patents
Method for extracting watermelon red coloring matter with assistance of floatation impurity removal Download PDFInfo
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- CN105038306A CN105038306A CN201510436933.XA CN201510436933A CN105038306A CN 105038306 A CN105038306 A CN 105038306A CN 201510436933 A CN201510436933 A CN 201510436933A CN 105038306 A CN105038306 A CN 105038306A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B61/00—Dyes of natural origin prepared from natural sources, e.g. vegetable sources
Abstract
The invention belongs to the field of food coloring matter preparation, and provides a method for extracting watermelon red coloring matter with the assistance of floatation impurity removal. The method includes the steps of (a) flesh removal, (b) beating, (c) coloring matter extraction, (d) crude coloring matter preparation, (e) coloring matter purification, (f) concentration drying and the like. In crude coloring matter preparation, extraction liquid is delivered into a floatation device, impurities are scraped off after flocculating and floating, and solid-liquid separation is achieved; then, vacuum concentration is performed on obtained separation liquid, freeze-drying is performed on concentrate, and crude coloring matter is obtained. The method has the advantages that by the adoption of membrane filtration, the energy consumption is low, and the yield is high; besides, the whole production process is easy to implement, low in equipment requirement and cost and quite suitable for industrial production; the obtained coloring matter is safe to eat and good in color and luster.
Description
Technical field
The invention belongs to food dye preparation field, relate to a kind of method extracting edible haematochrome.
Background technology
Natural pigment is the food dye obtained by natural resource.The main pigment extracted from animal and plant tissue and microorganism (cultivation), wherein vegetalitas tinting material occupies the majority.Natural pigment not only has to the effect of food color, and considerable part natural pigment has physiologically active.In the development & application of natural pigment, Japan occupy prostatitis, the world, and the usage quantity as far back as natural pigment in 1975 just exceedes synthetic colour.In China's natural food colour product, the output of time caramel colorant is maximum, and annual production accounts for 86% of natural food colour, is mainly used in domestic brewing industry and drink industry.Along with the further raising of our people's standard of living, the product of All Pure Nature raw material of going back to nature-eat will become the main flow of food consumption from now on, domestic food production will constantly increase the demand of natural food colour, also will open up the Application Areas that natural pigment is more wide in medicine-daily use chemicals etc. simultaneously.
Watermelon haematochrome belongs to the one in numerous food dye, and its pigment is bright-coloured, safety non-toxic, has wide market potential.But the extraction process of watermelon haematochrome is still the experimental phase at present, can only produce on a small scale pole.Existing watermelon haematochrome extracting method generally comprises following steps: watermelon, and------------dry---------------wash-out---concentrates---drying---freezen protective to macroporous resin adsorption in removal of impurities to get supernatant liquid to add pigment extraction agent in filtration in making beating to get capsule.Some contrivers have carried out the research of watermelon haematochrome extracting method, as:
The extraction of [autograph] watermelon haematochrome and anti-oxidant activity research [periodical name] Agricultural University of the Inner Mongol's journal [author] Zhang Meizhi-Huanghai Sea English-Zou Yin-Li Zhengying-Zhou Qun [date issued] in January, 2013 [synopsis] this research disclose a kind of extracting method of watermelon haematochrome: clean watermelon surface, get wooden dipper and remove seed, pull an oar with high-speed tissue mashing machine, through filtered through gauze, centrifugal (4000r/min, 10min), precipitation is dry with vacuum freeze drier.Take 2.00g Exocarpium Citrulli lyophilized powder, be placed in Erlenmeyer flask, add people 20mL acetone, connect reflux, lixiviate 3 times under 50 DEG C of conditions, 1h/ time, extract watermelon haematochrome, centrifugal (4000r/min, lOmin), supernatant liquor is concentrated by rotavapor under vacuum, dissolves with appropriate distilled water.On aqueous phase, D-101 macroporous adsorption resin chromatography post, first washes impurity with water, then utilizes mixed solution (2:1) the leacheate wash-out of acetone and acetic acid ethyl ester, obtains the watermelon haematochrome solution of purifying.
Mainly there is following shortcoming in existing watermelon red pigment extraction process: 1. make chemically removal of impurities, production cost is too high, reduces pigment edible safety simultaneously; 2. some processes adopts the toxic substances such as acetone, is unfavorable for that production operator is healthy.
Summary of the invention
The object of the invention is the shortcoming and defect overcoming the existence of existing watermelon red pigment extraction process, the edible haematochrome extracting method that a kind of cost is low, simple to operate, Product Safety is good is provided.
A method for the removal of impurities assisted extraction that floats watermelon haematochrome, comprises the step of getting flesh-making beating-pigment lixiviate-prepare pigment crude product-pigment pufification-concentrate drying, and prepare pigment crude product process and adopt floating method removal of impurities, concrete operation step is as follows:
A. flesh is got: from fresh watermelon, take out flesh of Pulp Citrulli;
B. pull an oar: flesh of Pulp Citrulli is carried out historrhexis and obtain flesh slurry, then filtered by flesh slurry, obtain Pulp Citrulli juice, filtering order number is 120-200;
C. pigment lixiviate: the ethanolic soln adding 65-75% in Pulp Citrulli juice, the volume ratio of Pulp Citrulli juice and ethanolic soln is 1:2-3, and lixiviate is got 2-3 time;
D. prepare pigment crude product: sent into by vat liquor in floating device, after impurity flocculation is floated, scrape the removal of impurity, realize solid-liquid separation; Again the parting liquid of gained is carried out vacuum concentration, lyophilize enriched material, obtain pigment crude product;
E. pigment pufification: pigment crude product liquid pigment crude product distilled water being mixed with 6.0-10.0g/L; Flow through macroporous adsorptive resins with the flow velocity of 0.2-2.5ml/min, carry out pigment absorption; Then with distilled water, macroporous adsorptive resins is rinsed, wash-out impurity; Use the ethanolic soln wash-out macroporous adsorptive resins of 65-75% again, obtain elutriant;
F. concentrate drying: elutriant is carried out concentrating under reduced pressure, obtains enriched material; Enriched material is carried out low-temperature vacuum drying, is dried to Powdered rear taking-up, obtains finished product pigment.
Wherein, the principle of floating method removal of impurities is: pass into bubble in solution after, and the impurity in small bubbles and solution meets and is adsorbed on contaminant surface; Along with the bubble of contaminant surface increases, the buoyancy that impurity is subject to increases gradually, finally floats to solution surface layer; When solution surface layer impurities accumulation to a certain extent after, just can strike off with dregs scraper, realize removal of impurities object.
The primary pigments digestion agent that the present invention adopts is the ethanolic soln of 65-75%, compares the organic reagents such as the high density acetone of conventional art use, has increased substantially pigment edible safety; Select 65-75% concentration ranges, not only meet the requirement of industrial lixiviate pigment, also reduce production cost.
Further illustrate as of the present invention, step c, in pigment leaching process, keep solution temperature between 5-10 DEG C.The temperature of pigment leaching process is important, keeps the temperature of 5-10 DEG C, can not be destroyed by available protecting pigment molecular.
Further illustrate as of the present invention, in step c and step e, ethanolic soln pH value used is 2.0-4.0.The pH value setting this scope destroys to prevent pigment molecular from suffering peracid or crossing alkali, ensures finished product color and luster.
Further illustrate as of the present invention, in steps d, it is 1-1.5h that floating device passes into the bubble time, and on average often liter of solution per minute passes into air 10-20L; A upper strata impurity is struck off every 10-15min.Practice shows, can remove the impurity of more than 80% after floating removal of impurities 1h, and the impurity-eliminating effect of 1.5h can reach more than 95%.
Further illustrate as of the present invention, in steps d, floating removal of impurities is gone in solution and is added the starch that feed liquid weight ratio is 1:80-120, stirs 5-10min.Starch itself is a kind of flocculation agent, has better adsorption to macromolecular substance most of in Pulp Citrulli juice, the composition such as pulp, suspended particle in the Pulp Citrulli juice that can flocculate; Add starch and carry out efficiency and the effect that floating removal of impurities can increase substantially removal of impurities again.
Further illustrate as of the present invention, in step e, the model of described macroporous adsorptive resins is HPD101, and its blade diameter length ratio is 1:10-20.Test proves that HPD101 type macroporous adsorptive resins is best to the haematochrome adsorption effect in Pulp Citrulli juice, can extract the pigment of in Pulp Citrulli juice about 90%.
Floating removal of impurities assisted extraction watermelon haematochrome method of the present invention compared with prior art has following progress:
1, adopt floating method removal of impurities, not only energy consumption low, pollute little, Yin Gaowen pigment can also be reduced and decompose, improve the rate of recovery.Practice shows, can remove the impurity of more than 80% after floating removal of impurities 1h, and the impurity-eliminating effect of 1.5h can reach more than 95%.
2, simple to operate, equipment requirements is low: production technique of the present invention only relates to gets flesh, making beating, pigment lixiviate, prepares the steps such as pigment crude product, pigment pufification, concentrate drying, performs simple fragmentation, stirring, floating removal of impurities, filtration, drying can complete pigment production and operate.
3, gained pigment edible safety, color and luster are good: primary pigments digestion agent is the ethanolic soln of 65-75%, not containing toxic substances such as acetone in finished product pigment, arsenic content <2ppm, lead content <1.5ppm, heavy metal content <13ppm; Finished product pigment purity reaches more than >90, bright color.
Embodiment
Technical scheme of the present invention is described in detail below in conjunction with embodiment.
Embodiment 1: a kind of method of the removal of impurities assisted extraction watermelon haematochrome that floats, concrete operation step is as follows:
A. flesh is got: from fresh watermelon, take out flesh of Pulp Citrulli;
B. pull an oar: flesh of Pulp Citrulli is carried out historrhexis and obtain flesh slurry, then filtered by flesh slurry, obtain Pulp Citrulli juice, filtering order number is 120-200;
C. pigment lixiviate: add the ethanolic soln of 65% in Pulp Citrulli juice, the volume ratio of Pulp Citrulli juice and ethanolic soln is 1:2, and lixiviate is got 2-3 time;
D. prepare pigment crude product: sent into by vat liquor in floating device, after impurity flocculation is floated, scrape the removal of impurity, realize solid-liquid separation; Again the parting liquid of gained is carried out vacuum concentration, lyophilize enriched material, obtain pigment crude product;
E. pigment pufification: pigment crude product liquid pigment crude product distilled water being mixed with 6.0g/L; Flow through macroporous adsorptive resins with the flow velocity of 0.2ml/min, carry out pigment absorption; Then with distilled water, macroporous adsorptive resins is rinsed, wash-out impurity; Use the ethanolic soln wash-out macroporous adsorptive resins of 65% again, obtain elutriant;
F. concentrate drying: elutriant is carried out concentrating under reduced pressure, obtains enriched material; Enriched material is carried out low-temperature vacuum drying, is dried to Powdered rear taking-up, obtains finished product pigment.
Embodiment 2: a kind of method of the removal of impurities assisted extraction watermelon haematochrome that floats, concrete operation step is as follows:
A. flesh is got: from fresh watermelon, take out flesh of Pulp Citrulli;
B. pull an oar: flesh of Pulp Citrulli is carried out historrhexis and obtain flesh slurry, then filtered by flesh slurry, obtain Pulp Citrulli juice, filtering order number is 200;
C. pigment lixiviate: add the ethanolic soln of 75% in Pulp Citrulli juice, the volume ratio of Pulp Citrulli juice and ethanolic soln is 1:-3, and lixiviate is got 2-3 time;
D. prepare pigment crude product: sent into by vat liquor in floating device, after impurity flocculation is floated, scrape the removal of impurity, realize solid-liquid separation; Again the parting liquid of gained is carried out vacuum concentration, lyophilize enriched material, obtain pigment crude product;
E. pigment pufification: pigment crude product liquid pigment crude product distilled water being mixed with 10.0g/L; Flow through macroporous adsorptive resins with the flow velocity of 2.5ml/min, carry out pigment absorption; Then with distilled water, macroporous adsorptive resins is rinsed, wash-out impurity; Use the ethanolic soln wash-out macroporous adsorptive resins of 75% again, obtain elutriant;
F. concentrate drying: elutriant is carried out concentrating under reduced pressure, obtains enriched material; Enriched material is carried out low-temperature vacuum drying, is dried to Powdered rear taking-up, obtains finished product pigment.
Embodiment 3: flesh of Pulp Citrulli is carried out historrhexis and obtain flesh slurry, then filtered by flesh slurry, obtain Pulp Citrulli juice, filtering order number is 120-200;
C. pigment lixiviate: add the ethanolic soln of 70% in Pulp Citrulli juice, the volume ratio of Pulp Citrulli juice and ethanolic soln is 1:2.5, and lixiviate gets 3 times;
D. prepare pigment crude product: sent into by vat liquor in floating device, after impurity flocculation is floated, scrape the removal of impurity, realize solid-liquid separation; Again the parting liquid of gained is carried out vacuum concentration, lyophilize enriched material, obtain pigment crude product;
E. pigment pufification: pigment crude product liquid pigment crude product distilled water being mixed with 8.0g/L; Flow through macroporous adsorptive resins with the flow velocity of 1.5ml/min, carry out pigment absorption; Then with distilled water, macroporous adsorptive resins is rinsed, wash-out impurity; Use the ethanolic soln wash-out macroporous adsorptive resins of 70% again, obtain elutriant;
F. concentrate drying: elutriant is carried out concentrating under reduced pressure, obtains enriched material; Enriched material is carried out low-temperature vacuum drying, is dried to Powdered rear taking-up, obtains finished product pigment.
Embodiment 4: a kind of method of the removal of impurities assisted extraction watermelon haematochrome that floats, its operation steps is substantially identical with embodiment 3, and unique difference is: step c, in pigment leaching process, keeps solution temperature between 5-10 DEG C.
Embodiment 5: a kind of method of the removal of impurities assisted extraction watermelon haematochrome that floats, its operation steps is substantially identical with embodiment 3, and unique difference is: in step c and step e, ethanolic soln pH value used is necessary for 2.0-4.0.
Embodiment 6: a kind of method of the removal of impurities assisted extraction watermelon haematochrome that floats, its operation steps is substantially identical with embodiment 3, and unique difference is: in step e, the model of described macroporous adsorptive resins is necessary for HPD101, and its blade diameter length ratio is 1:10-20.
Embodiment 7: a kind of method of the removal of impurities assisted extraction watermelon haematochrome that floats, its operation steps is substantially identical with embodiment 3, and unique difference is: in steps d, it is 1-1.5h that floating device passes into the bubble time, and on average often liter of solution per minute passes into air 10-20L; A upper strata impurity is struck off every 10-15min.
Embodiment 8: a kind of method of the removal of impurities assisted extraction watermelon haematochrome that floats, its operation steps is substantially identical with embodiment 3, and unique difference is: in steps d, floating removal of impurities is gone in solution and added the starch that feed liquid weight ratio is 1:80-120, stirs 5-10min.
Specificity analysis discovery is carried out to the pigment finished product of embodiment 7 gained:
Find through solvent solubility experiment: watermelon haematochrome is water colo(u)r, dissolves in methyl alcohol, ethanol, acetone polar organic solvent, and can not be dissolved in the non-polar organic solvents such as benzene, chloroform, sherwood oil.
Find through cold and hot stability experiment: very large on the impact of watermelon haematochrome from the cold and hot stability experiment temperature of watermelon haematochrome, the freezing change that substantially can not cause watermelon haematochrome extracting solution color and luster, shows freezing can not damaging its pigmentary structures.And fugitive color becomes glassy yellow after being heated, acid adding or to add alkali all irreversible, shows that pigmentary structures is destroyed.Therefore watermelon haematochrome thermotolerance is poor.
Below the implementation result of different embodiment is described:
When the technique of different embodiment expends, there is certain difference in the aspect such as operation easier, pigment extraction yield, total production cost, final product quality, specifically as shown in table 1:
Also there is certain difference in the quality product of different embodiment, specifically as shown in table 2:
In general, the present invention floats the method for removal of impurities assisted extraction watermelon haematochrome, and simple to operate, equipment requirements is low, with low cost, is very suitable for industrial production.Gained pigment finished product edible safety, indices is good.
Claims (6)
1. the method for removal of impurities assisted extraction watermelon haematochrome that floats, comprise the step of getting flesh-making beating-pigment lixiviate-prepare pigment crude product-pigment pufification-concentrate drying, it is characterized in that described pigment crude product process of preparing adopts floating method removal of impurities, concrete operation step is as follows:
A. flesh is got: from fresh watermelon, take out flesh of Pulp Citrulli;
B. pull an oar: flesh of Pulp Citrulli is carried out historrhexis and obtain flesh slurry, then filtered by flesh slurry, obtain Pulp Citrulli juice, filtering order number is 120-200;
C. pigment lixiviate: the ethanolic soln adding 65-75% in Pulp Citrulli juice, the volume ratio of Pulp Citrulli juice and ethanolic soln is 1:2-3, and lixiviate is got 2-3 time;
D. prepare pigment crude product: sent into by vat liquor in floating device, after impurity flocculation is floated, scrape the removal of impurity, realize solid-liquid separation; Again the parting liquid of gained is carried out vacuum concentration, lyophilize enriched material, obtain pigment crude product;
E. pigment pufification: pigment crude product liquid pigment crude product distilled water being mixed with 6.0-10.0g/L; Flow through macroporous adsorptive resins with the flow velocity of 0.2-2.5ml/min, carry out pigment absorption; Then with distilled water, macroporous adsorptive resins is rinsed, wash-out impurity; Use the ethanolic soln wash-out macroporous adsorptive resins of 65-75% again, obtain elutriant;
F. concentrate drying: elutriant is carried out concentrating under reduced pressure, obtains enriched material; Enriched material is carried out low-temperature vacuum drying, is dried to Powdered rear taking-up, obtains finished product pigment.
2. the method for floating removal of impurities assisted extraction watermelon haematochrome according to claim 1, is characterized in that: step c, in pigment leaching process, keeps solution temperature between 5-10 DEG C.
3. the method for floating removal of impurities assisted extraction watermelon haematochrome according to claim 1, it is characterized in that: in step c and step e, ethanolic soln pH value used is 2.0-4.0.
4. the method for floating removal of impurities assisted extraction watermelon haematochrome according to claim 1, it is characterized in that: in steps d, it is 1-1.5h that floating device passes into the bubble time, and on average often liter of solution per minute passes into air 10-20L; A upper strata impurity is struck off every 10-15min.
5. the method for floating removal of impurities assisted extraction watermelon haematochrome according to claim 1, it is characterized in that: in steps d, floating removal of impurities is gone in solution and is added the starch that feed liquid weight ratio is 1:80-120, stirs 5-10min.
6. the method for floating removal of impurities assisted extraction watermelon haematochrome according to claim 1, it is characterized in that: in step e, the model of described macroporous adsorptive resins is HPD101, and its blade diameter length ratio is 1:10-20.
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