CN103740130A - Preparation method of gardenia yellow pigment - Google Patents
Preparation method of gardenia yellow pigment Download PDFInfo
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Abstract
The invention discloses a preparation method of a gardenia yellow pigment. The method comprises the following steps: 1, carrying out enzymolysis on gardenia raw materials for 1-3 times by using a composite enzyme preparation, so that an extracting solution is obtained; 2, carrying out adsorption refining on the extracting solution by using macroporous adsorption resins so as to obtain a refining solution, and concentrating the refining solution so as to obtain a concentrated cream; 3, crystallizing the concentrated cream by using a crystallization solvent, so that a gardenia yellow pigment product is obtained. According to the method provided by the invention, the pigment loss caused by the manufacturing procedure and the number of times of concentrating is reduced, the quality of obtained products is good, the energy consumption is low, and the method is convenient for industrial production.
Description
Technical field
The present invention relates to a kind of preparation method of Gardenia Yellow.
Background technology
In Rubiaceae (Rubiaceae) plant cape jasmine (Gardenia jasminoides Ellis), contained Gardenia Yellow is natural water-soluble carotenoid, and its main component comprises Crocin, trans-crocetin and jasminoidin.
In prior art, the preparation of Gardenia Yellow is mainly to adopt extraction using alcohol, after reclaiming ethanol, use Macroporous Adsorption Resin pigment, the Gardenia Yellow that need to carry out successively again that secondary concentration, membrane filtration, three times are concentrated, spraying and drying step obtains powdery, existing Gardenia Yellow preparation method's production process is loaded down with trivial details, ethanol loss is large, production cost is high, the Gardenia Yellow of acquisition
Therefore be necessary to provide that a kind of operation is easy, production cost is low, can obtain the Gardenia Yellow preparation method of high-quality Gardenia Yellow product.
Summary of the invention
The object of the invention is to overcome that the operation existing in existing Jasmin uranidin prodn. tech is loaded down with trivial details, production cost is high, the shortcoming of poor product quality, provides that a kind of can to obtain jasminoidin foreign matter content low, Gardenia Yellow
and the new Gardenia Yellow production method that the easy cost consumption of operation is low.
For reaching above object, the invention provides a kind of preparation method of Gardenia Yellow, wherein, the method comprises the following steps:
Step 1: with compound enzymic preparation, cape jasmine raw material is carried out to 1-3 enzymolysis and obtain extracting solution;
Step 2: with macroporous adsorbent resin, described extracting solution is carried out to refining with adsorbents, obtain refined liquid, and described refined liquid is concentrated, obtain condensed cream;
Step 3: with recrystallisation solvent, condensed cream is carried out to crystallization, obtain Gardenia Yellow product.
First method provided by the present invention is used containing a certain amount of compound extraction enzyme aqueous solution and is extracted, prozyme extracts has specificity and high efficiency, by the method, improved extraction yield and efficiency, after traditional process for purification, re-used mixed solvent crystallization and process, obtained
be 850, low Determination of Gardenoside (with
meter is less than 0.007%) Gardenia Yellow, the good product quality, the energy consumption that reduced pigment loss that manufacturing procedure and concentrated number of times bring, obtain be low, be convenient to suitability for industrialized production.
Embodiment
Below the specific embodiment of the present invention is elaborated.Should be understood that, embodiment described herein only, for description and interpretation the present invention, is not limited to the present invention.
The invention provides a kind of preparation method of Gardenia Yellow, wherein, the method comprises the following steps:
Step 1: with compound enzymic preparation, cape jasmine raw material is carried out to 1-3 enzymolysis and obtain extracting solution;
Step 2: with macroporous adsorbent resin, described extracting solution is carried out to refining with adsorbents, obtain refined liquid, and described refined liquid is concentrated, obtain condensed cream;
Step 3: with recrystallisation solvent, condensed cream is carried out to crystallization, obtain Gardenia Yellow product.
Wherein, described cape jasmine raw material is for pulverizing the fruit of madder wort Rubiaceae (Rubiaceae) plant cape jasmine (Gardenia jasminoides Ellis) cross the feed particles that 10 mesh sieves obtain.
In method provided by the present invention, described compound enzymic preparation selects one or more in the group that free cellulase, hemicellulase, polygalacturonase, proteolytic enzyme, Lipase and amylase forms.
In preferred situation, described compound enzymic preparation comprises cellulase, hemicellulase, polygalacturonase, proteolytic enzyme, Lipase and amylase.
In preparation method provided by the present invention, the enzyme that described cellulase can have a cellulose degradation ability by zytase and beta-glucosidase etc. forms, the cellulase using in the present invention can be the commercially available cellulase finished product bought cellulose complex enzyme finished product for example, preferably, described cellulase is the prozyme finished product of beta-glucanase, zytase and glucuroide.In the method providing in invention, described beta-glucanase is preferably beta-glucanase 1,4 excision enzymes.
In preparation method provided by the present invention, the enzyme that described hemicellulase can have a hemicellulose degradation capability by xylosidase, arabinoxylanase, glucuroide, mannase and tilactase etc. forms, wherein arabinoxylanase comprises inscribe β-1, one or more in 4-D zytase (EC3.2.1.8), circumscribed β-Isosorbide-5-Nitrae-zytase (EC3.2.1.37) and xylobiase.The hemicellulase using in the present invention can be the commercially available hemicellulase finished product of buying, for example hemicellulose prozyme finished product.Preferably, described hemicellulase selects one or more in the group that free xylosidase, arabinoxylanase, glucuroide, mannase and tilactase form.
In preparation method provided by the present invention, the enzyme that described polygalacturonase can have a pectin degrading ability by protopectinase, pectinesterase lytic enzyme, polygalacturonase class and pectate lyase etc. forms, the polygalacturonase using in the present invention can be the commercially available polygalacturonase finished product of buying, for example polygalacturonase prozyme finished product.
Preferably, described polygalacturonase selects one or more in the group that free protopectinase, pectinesterase lytic enzyme, polygalacturonase and pectin lyase form.
In preparation method provided by the present invention, described proteolytic enzyme can be in thiol proteinase, aspartate protease, serine/threonine protein enzyme and metalloprotease etc. can enzymolysis cape jasmines the enzyme of protein matter form, the proteolytic enzyme using in the present invention can be the commercially available proteolytic enzyme finished product of buying, for example protease composite enzyme finished product.Preferably, described proteolytic enzyme is one or more in thiol proteinase, aspartate protease, serine/threonine protein enzyme and metalloprotease.
In preparation method provided by the present invention, and described Lipase (No. CAS: 9001-62-1) can make fat splitting is lipid acid and glycerine, generate lipid acid, glycerine and monoglyceride or diester.
In preparation method provided by the present invention, amylase can be comprised of α-powder amylase, β-powder enzyme, gamma amylase, isoamylase, the starch in can enzymolysis cape jasmine such as amylase and the enzyme of glycogen form, the amylase using in the present invention can be the commercially available amylase finished product of buying, for example amylase prozyme finished product.One or more in α-amylase, beta-amylase, γ-powder amylase and isoamylase preferably.
In preparation method provided by the present invention; cape jasmine raw material with respect to 1000 grams, the consumption of the cellulase that each enzymolysis adds is that the consumption of 2000-20000 unit, hemicellulase is that the consumption of 2000-20000 unit, polygalacturonase is that the consumption of 1000-5000 unit, proteolytic enzyme is that the consumption of 1000-10000 unit, Lipase is that 1000-20000 unit, diastatic consumption are 1000-10000 unit.
In preferred situation; cape jasmine raw material with respect to 1000 grams; the consumption of the cellulase that each enzymolysis adds is that the consumption of 5000-10000 unit, hemicellulase is that the consumption of 5000-10000 unit, polygalacturonase is 2000-4500 unit, and the consumption of proteolytic enzyme is that the consumption of 5000-9500, Lipase is that 5000-9500 unit, diastatic consumption are 3000-5000 unit.
In preparation method's provided by the present invention step 1, can adopt the method for primary enzymolysis to obtain extracting solution, also can adopt repeatedly the method for united extraction liquid after enzymolysis to carry out extraction process to cape jasmine raw material, method provided by the present invention preferably adopts the method for three enzymolysis to carry out, and three enzymolysis and extraction liquid are merged and obtain total extracting solution.
In the present invention, with acetic acid-sodium acetate buffer of 10 volume %-20 volume %, regulate the pH value of water to 4.0-5.0.The concentration of described acetic acid-sodium acetate buffer can be for 10 volume %-20 volume %, and with respect to the cape jasmine raw material of 1000g, the amount of the water that each enzymolysis adds is 2000-3500ml, is preferably 2500-3000ml.
In method provided by the present invention, can collect extracting solution by the method for filtering, filter filter screen used for being not less than 400 orders, filtration filter paper is Medium speed filter paper.
In method provided by the present invention, the condition of described enzymolysis is, temperature 25-40 ℃, pH value 4.0-5.0, each enzymolysis stirs and extracts 0.5-1.5h, and in preferred situation, the condition of described enzymolysis is, temperature 35-40 ℃, pH value 4.5-5.0, each enzymolysis stirs and extracts 1.2-1.5h.
Method provided by the present invention also comprises with macroporous adsorbent resin carries out refining with adsorbents to extracting solution, in method provided by the present invention, kind to described macroporous adsorbent resin has no particular limits, can be conventional any one macroporous adsorbent resin using in this area, for example described macroporous adsorbent resin can be selected from one or more in LSA-10, LSA-2, LS-300.
In the present invention, to adsorb the exquisite refined liquid obtaining by macroporous adsorbent resin, carry out concentrated method and have no particular limits, can adopt this area to refine the method that enrichment step is conventional and carry out, in preferred situation, described refining process comprises:
Resin pre-treatment: get 500mL resin, by alkali and 95 volume % alcohol process resin, process that to add water to ethanol limpid; Water rushes to alcohol-free to be used.
Absorption: adsorptive capacity 15BV, absorption flow velocity 1BV/h, direction upper entering and lower leaving.
Washing: water consumption 10BV, flow velocity 1BV/h, direction upper entering and lower leaving.
Desorb: 60 volume % ethanol desorbs, consumption 1BV, flow velocity 0.5BV/h, direction upper entering and lower leaving.
Refined liquid is concentrated: merge three refined liquid and concentrate.The condensed cream obtaining
be more than or equal to 150.
Method provided by the present invention also comprises carries out further crystallization treatment to condensed cream, the method of described crystallization treatment is: the condensed cream that step 2 is obtained is dissolved in recrystallisation solvent, at 0-5 ℃, after standing 36-60h, filter and obtain coarse crystallization filter cake, at 0-5 ℃, with recrystallisation solvent washing coarse crystallization filter cake, obtain xln again, the xln of acquisition dry 3-4h under temperature 60-65 ℃, vacuum tightness 0.07-0.08MPa obtains Gardenia Yellow product.
Wherein, with respect to the condensed cream of 100g, for dissolving the consumption of the recrystallisation solvent of condensed cream, be 300-450ml, for washing the consumption of the recrystallisation solvent of coarse crystallization filter cake, be 100-200ml; In preferred situation, for dissolving the consumption of the recrystallisation solvent of condensed cream, being 350-390ml, is 100-120ml for washing the consumption of the recrystallisation solvent of coarse crystallization filter cake.
In method provided by the present invention, can adopt the mixing solutions of ethanol or ethanol and ethyl acetate to carry out crystallization to condensed cream, preferably, described recrystallisation solvent is the mixing solutions of ethanol and ethyl acetate, when described recrystallisation solvent is the mixing solutions of ethanol and ethyl acetate, the volume ratio of ethanol and ethyl acetate is 2.3-3.0:1, is preferably 2.3-2.4:1.
In the present invention, the ethanol that described ethanol is food grade, purity is 95-96 volume %, the ethyl acetate that described ethyl acetate is food grade, purity is 98-99 volume %.
In step 3, can adopt the method for suction filtration to obtain coarse crystallization filter cake, in order further to improve the purity of Gardenia Yellow product, need to filter cake, carry out further washing to remove impurity and the mother liquor in coarse crystallization filter cake with recrystallisation solvent, the method for washing can be for carrying out drip washing with recrystallisation solvent to filter cake.
Below will describe the present invention by embodiment.In following examples,
Cape jasmine fruit is pulverized and crossed 10 mesh sieves and obtain cape jasmine raw material.
Cellulase compound enzymic preparation is purchased from jade of the He family biotechnology company limited.Bai Wei bio tech ltd, Hebei; hemicellulase compound enzymic preparation is purchased from jade of the He family biotechnology company limited; polygalacturonase compound enzymic preparation is purchased from jade of the He family biotechnology company limited; protease composite enzyme preparation is purchased from jade of the He family biotechnology company limited; Lipase is purchased from jade of the He family biotechnology company limited; amylase is purchased from jade of the He family biotechnology company limited, and in the present invention, the moiety of each prozyme is in Table 1.This patent is respectively LSA-10, LSA-20, LS-300 with resin, and resin is purchased from Shaanxi Lan Shen Special Resin company limited.
In the present invention:
The detection method of look valency is carried out according to the method for defined in GB79122010.
The detection method of jasminoidin is carried out according to the method for defined in GB79122010.
Table 1
Embodiment 1
According to the listed ratio of table 2, in 1000g cape jasmine raw material, add pure water and compound enzymic preparation to obtain extraction system, pH value to 4.6 by acetic acid-sodium acetate regulation system, at the extraction temperature of 37 ℃, with the mixing speed of 300 revs/min, extract 1.3h, after filtering acquisition extracting solution with 400 mesh sieves, under identical extraction conditions, extract 2 times again, the extracting solution of three times is merged and obtains Medium speed filter paper and filter and to obtain total extracting solution 8500g, and extracting solution is crossed Medium speed filter paper, filtrate collection; Extracting solution
be 2.43; With LSA-10 macroporous adsorbent resin, 500mL refines extracting solution: absorption: adsorptive capacity 8.5BV, absorption flow velocity 1BV/h, direction upper entering and lower leaving.Washing: water consumption 10BV, flow velocity 1BV/h, direction upper entering and lower leaving.Desorb: 60 volume % ethanol desorbs, consumption 1BV, flow velocity 0.5BV/h, direction upper entering and lower leaving.Refined liquid is to be concentrated: merge twice refined liquid to be concentrated; Obtain refined liquid, refined liquid
be 14.21; Refined liquid is concentrated into
be 150, obtain 130g condensed cream; With 380ml recrystallisation solvent (ethanol: ethyl acetate=2.3:1 (v/v)), condensed cream is diluted to standing 36h under the temperature condition of 3 ℃; Crystallization time obtains crystallization coarse filtration cake to rear with filter flask suction filtration, then with 110ml recrystallisation solvent (ethanol: ethyl acetate=2.3:1 (v/v)) washing coarse filtration cake, obtains xln at 3 ℃; Xln is put into baking oven in 63 ℃, dry 3.5h under vacuum tightness 0.075MPa condition, obtains Gardenia Yellow product 20.46g again.
Detect look valency and the glycosides content of Gardenia Yellow product: crest 443.50,
be 850.43, Determination of Gardenoside with
count 0.0061%.
Embodiment 2
According to the listed ratio of table 2, in 1000g cape jasmine raw material, add pure water and compound enzymic preparation to obtain extraction system, pH value to 4.8 by acetic acid-sodium acetate regulation system, at the extraction temperature of 35 ℃, with the mixing speed of 300 revs/min, extract 1.2h, after filtering acquisition extracting solution with 400 mesh sieves, under identical extraction conditions, extract 2 times again, the extracting solution of three times is merged to Medium speed filter paper and filter the total extracting solution 8535g of acquisition, extracting solution is crossed Medium speed filter paper, filtrate collection; Extracting solution
be 2.30; With LSA-20 macroporous adsorbent resin, 500mL refines extracting solution: absorption: adsorptive capacity 8.84BV, absorption flow velocity 1BV/h, direction upper entering and lower leaving.Washing: water consumption 10BV, flow velocity 1BV/h, direction upper entering and lower leaving.Desorb: 60 volume % ethanol desorbs, consumption 1BV, flow velocity 0.5BV/h, direction upper entering and lower leaving; Obtain refined liquid, refined liquid
be 13.39; Refined liquid is concentrated into
be 153.25, obtain 128.5g condensed cream; With 350ml recrystallisation solvent (ethanol: ethyl acetate=2.5:1 (v/v)), condensed cream is diluted to standing 48h under the temperature condition of 2 ℃; Crystallization time obtains crystallization coarse filtration cake to rear with filter flask suction filtration, then with 100ml recrystallisation solvent (ethanol: ethyl acetate=2.5:1 (v/v)) washing coarse filtration cake, obtains xln at 2 ℃; Xln is put into baking oven in 63 ℃, dry 3h under vacuum tightness 0.08MPa condition, obtains Gardenia Yellow product 20.36g again.
Detect look valency and the glycosides content of Gardenia Yellow product: crest 444.50,
be 854.35, Determination of Gardenoside with
count 0.0063%.
Embodiment 3
According to the listed ratio of table 2, in 1000g cape jasmine raw material, add pure water and compound enzymic preparation to obtain extraction system, pH value to 4.5 by acetic acid-sodium acetate regulation system, at the extraction temperature of 39 ℃, with the mixing speed of 300 revs/min, extract 1.4h, after filtering acquisition extracting solution with 400 mesh sieves, under identical extraction conditions, extract 2 times again, the extracting solution of three times is merged to Medium speed filter paper and filter the total extracting solution 9500g of acquisition, extracting solution is crossed Medium speed filter paper, filtrate collection; Extracting solution
be 2.30; With LS-300 macroporous adsorbent resin, 500mL refines extracting solution: absorption: adsorptive capacity 9.5BV, absorption flow velocity 1BV/h, direction upper entering and lower leaving.Washing: water consumption 10BV, flow velocity 1BV/h, direction upper entering and lower leaving.Desorb: 60 volume % ethanol desorbs, consumption 1BV, flow velocity 0.5BV/h, direction upper entering and lower leaving; Obtain refined liquid, refined liquid
be 13.14; Refined liquid is concentrated into
be 156.38, obtain 126.1g condensed cream; With 390ml recrystallisation solvent (ethanol: ethyl acetate=2.8:1 (v/v)), condensed cream is diluted to standing 36h under the temperature condition of 4 ℃; Crystallization time obtains crystallization coarse filtration cake to rear with filter flask suction filtration, then with 120ml recrystallisation solvent (ethanol: ethyl acetate=2.8:1 (v/v)) washing coarse filtration cake, obtains xln at 4 ℃; Xln is put into baking oven in 65 ℃, dry 4h under vacuum tightness 0.07MPa condition, obtains Gardenia Yellow product 20.06g again.
Detect look valency and the glycosides content of Gardenia Yellow product: crest 442.50,
be 853.29, Determination of Gardenoside with
count 0.0065%.
Embodiment 4
According to the listed ratio of table 2, in 1000g cape jasmine raw material, add pure water and compound enzymic preparation to obtain extraction system, pH value to 4.2 by acetic acid-sodium acetate regulation system, at the extraction temperature of 28 ℃, with the mixing speed of 300 revs/min, extract 0.8h, after filtering acquisition extracting solution with 400 mesh sieves, under identical extraction conditions, extract 2 times again, the extracting solution of three times is merged to Medium speed filter paper and filter the total extracting solution 8510g of acquisition, extracting solution is crossed Medium speed filter paper, filtrate collection; Extracting solution
be 2.40; With LSA-10 macroporous adsorbent resin, 500mL refines extracting solution: absorption: adsorptive capacity 8.5BV, absorption flow velocity 1BV/h, direction upper entering and lower leaving.Washing: water consumption 10BV, flow velocity 1BV/h, direction upper entering and lower leaving.Desorb: 60 volume % ethanol desorbs, consumption 1BV, flow velocity 0.5BV/h, direction upper entering and lower leaving; Obtain refined liquid, refined liquid
be 13.14; Refined liquid is concentrated into
be 156.38, obtain 125.1g condensed cream; With 300ml recrystallisation solvent (95 volume % ethanol), condensed cream is diluted to standing 24h under the temperature condition of 0 ℃; Crystallization time obtains crystallization coarse filtration cake to rear with filter flask suction filtration, then with 100ml recrystallisation solvent (ethanol: ethyl acetate=2.3:1 (v/v)) washing coarse filtration cake, obtains xln at 0 ℃; Xln is put into baking oven in 60 ℃, dry 4h under vacuum tightness 0.08MPa condition, obtains Gardenia Yellow product 20.16g again.
Detect look valency and the glycosides content of Gardenia Yellow product: crest 442.50,
be 869.29, Determination of Gardenoside with
count 0.0069%.
Embodiment 5
According to the listed ratio of table 2, in 1000g cape jasmine raw material, add pure water and compound enzymic preparation to obtain extraction system, pH value to 4.9 by acetic acid-sodium acetate regulation system, at the extraction temperature of 40 ℃, with the mixing speed of 300 revs/min, extract 1.5h, after filtering acquisition extracting solution with 400 mesh sieves, under identical extraction conditions, extract 2 times again, the extracting solution of three times is merged to Medium speed filter paper and filter the total extracting solution 9500g of acquisition, extracting solution is crossed Medium speed filter paper, filtrate collection; Extracting solution
be 2.32; With LS-300 macroporous adsorbent resin, 500mL refines extracting solution: absorption: adsorptive capacity 9.5BV, absorption flow velocity 1BV/h, direction upper entering and lower leaving.Washing: water consumption 10BV, flow velocity 1BV/h, direction upper entering and lower leaving.Desorb: 60 volume % ethanol desorbs, consumption 1BV, flow velocity 0.5BV/h, direction upper entering and lower leaving; Obtain refined liquid, refined liquid
be 13.14; Refined liquid is concentrated into
be 157.38, obtain 126.1g condensed cream; With 450ml recrystallisation solvent (95 volume % ethanol), condensed cream is diluted to standing 30h under the temperature condition of 5 ℃; Crystallization time obtains crystallization coarse filtration cake to rear with filter flask suction filtration, then carries at 5 ℃ with 200ml recrystallisation solvent (ethanol: ethyl acetate=2.3:1 (v/v)) washing coarse filtration cake acquisition xln; Xln is put into baking oven in 64 ℃, dry 4h under vacuum tightness 0.07MPa condition, obtains Gardenia Yellow product 20.11g again.
Detect look valency and the glycosides content of Gardenia Yellow product: crest 442.50,
be 867.29, Determination of Gardenoside with
count 0.0068%.
Table 2
Comparative example 1
This comparative example is used for illustrating existing Gardenia Yellow preparation method.
In 1000g cape jasmine raw material, add 50 volume % extraction using alcohols twice, extracting temperature is 35 ℃, and each consumption 3000mL crosses Medium speed filter paper and obtains extracting solution, obtains filtrate 5300g, filtrate
be 4.12, concentrated 3 times of thick cream 1766g of acquisition, the thick cream doubly measured
be 12.37; Add water 2603g and be diluted to 4369 and stir, the diluent of acquisition
be 5; With Medium speed filter paper, filter, collect filtrate.With LS-300 macroporous adsorbent resin, 500mL refines: absorption, adsorptive capacity 4.4BV, absorption flow velocity 0.5BV/h, direction upper entering and lower leaving; Washing: water consumption 10BV, flow velocity 1BV/h, direction upper entering and lower leaving.Gradient desorption: 20 volume % ethanol desorbs, consumption 1BV, direction upper entering and lower leaving, flow velocity 0.5BV/h, treats that 20 volume % ethanol are finished to revealing resin, with 60 volume % ethanol desorbs, consumption 1BV, flow velocity 0.5BV/h, direction upper entering and lower leaving, obtains refined liquid; Refined liquid is divided 20 volume % ethanol part 500g,
for 2.2(collects as raffinate), 60 volume % ethanol refined liquid 1500g,
be 13.11, for concentrated, concentrate and doubly measure 3 times, 60 volume % ethanol cream 500g,
be 39.3; 0-5 ℃ of sedimentation 24h of 60 volume % ethanol cream, the time is centrifugal to rear taking-up supernatant liquor, centrifugate 450g,
be 40, centrifugate adds pure water 3150g to 3600g,
be 5, claim centrifugal diluent; The membrane concentration of molecular weight cut-off 6000 for centrifugal diluent, obtains filtrate 3000g, concentrated solution 600g,
be 25, the heating of membrane concentration liquid is concentrated into
be 150.38, weight 99g essence cream, smart cream is put into baking oven in 64 ℃, and dry 6h under vacuum tightness 0.07MPa condition, obtains Gardenia Yellow product 30.30g.
Detect look valency and the glycosides content of Gardenia Yellow product: crest 442.50,
be 495.05, Determination of Gardenoside with
count 0.0463%.
From the result of above embodiment, can find out, by method provided by the present invention, can prepare look valency
be not less than 850 Gardenia Yellow product, and the content of jasminoidin impurity with
meter is lower than 0.007%
By embodiment 1 is compared and can be found out with comparative example 1, method provided by the present invention has been reduced a plurality of preparation sections, and concentrated number of times has reduced twice, more easily operation, from extracting solution to powder, the yield of Gardenia Yellow is 84.24%, product quality aspect: crest 443.50
850.43, Determination of Gardenoside with
count 0.0061%, and comparative example 1 operation sequence is more, concentrated number of times is more, from extracting solution to powder Gardenia Yellow yield: 68.69%.Product quality: crest 442.50,
determination of Gardenoside with
count 0.0463%.
More than describe the preferred embodiment of the present invention in detail; but the present invention is not limited to the detail in above-mentioned embodiment, within the scope of technical conceive of the present invention; can carry out multiple simple variant to technical scheme of the present invention, these simple variant all belong to protection scope of the present invention.It should be noted that in addition, each concrete technical characterictic described in above-mentioned embodiment, in reconcilable situation, can combine for fear of unnecessary repetition by any suitable mode, the present invention is to the explanation no longer separately of various possible array modes.
In addition, between various embodiment of the present invention, also can carry out arbitrary combination, as long as it is without prejudice to thought of the present invention, it should be considered as content disclosed in this invention equally.
Claims (10)
1. a preparation method for Gardenia Yellow, is characterized in that, the method comprises the following steps:
Step 1: with compound enzymic preparation, cape jasmine raw material is carried out to 1-3 enzymolysis and obtain extracting solution;
Step 2: with macroporous adsorbent resin, described extracting solution is carried out to refining with adsorbents, obtain refined liquid, and described refined liquid is concentrated, obtain condensed cream;
Step 3: with recrystallisation solvent, condensed cream is carried out to crystallization, obtain Gardenia Yellow product.
2. preparation method according to claim 1; wherein, described compound enzymic preparation selects one or more in the group that free cellulase, hemicellulase, beta-glucanase, polygalacturonase, proteolytic enzyme, Lipase and amylase forms.
3. preparation method according to claim 1 and 2; wherein; cape jasmine raw material with respect to 1000 grams, the consumption of the cellulase that each enzymolysis adds is that the consumption of 2000-20000 unit, hemicellulase is that the consumption of 2000-20000 unit, polygalacturonase is that the consumption of 1000-10000 unit, proteolytic enzyme is that the consumption of 1000-10000 unit, Lipase is that 1000-10000 unit, diastatic consumption are 1000-10000 unit.
4. preparation method according to claim 1 and 2, wherein, the condition of described enzymolysis is, with acetic acid-sodium acetate buffer of 10 volume %-20 volume %, regulates the pH value of water to 4.0-5.0, in temperature, is at 25-40 ℃, to stir to extract 0.5-1.5h.
5. according to the preparation method described in claim 2 or 4, wherein, in step 1, with respect to the cape jasmine raw material of 1000g, the amount of the water that each enzymolysis adds is 2000-3500ml.
6. preparation method according to claim 1 and 2, wherein, the method of described crystallization is: condensed cream is dissolved in recrystallisation solvent, at 0-5 ℃, after standing 36-60h, filter and obtain coarse crystallization filter cake, at 0-5 ℃, with recrystallisation solvent washing coarse crystallization filter cake, obtain xln, then by xln dry Gardenia Yellow product that obtains under temperature 60-65 ℃, vacuum tightness 0.07-0.08MPa.
7. preparation method according to claim 6, wherein, described recrystallisation solvent is the ethanolic soln of 95 volume % or is the mixing solutions of ethanol and ethyl acetate.
8. preparation method according to claim 7, wherein, when described recrystallisation solvent is the mixing solutions of ethanol and ethyl acetate, the volume ratio of ethanol and ethyl acetate is 2.3-3.0:1.
9. preparation method according to claim 6, wherein, with respect to the condensed cream of 100g, is 300-450ml for dissolving the consumption of the recrystallisation solvent of condensed cream, for washing the consumption of the recrystallisation solvent of coarse crystallization filter cake, is 150-200ml.
10. according to the preparation method described in any one in claim 1,2,7-9, wherein, described condensed cream
be more than or equal to 150.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108558645A (en) * | 2018-05-18 | 2018-09-21 | 武汉雅仕博科技有限公司 | The method that crocin is extracted from cape jasmine |
| CN108774407A (en) * | 2018-05-30 | 2018-11-09 | 山东省农业科学院农产品研究所 | A kind of extracting method of gardenia yellow pigment with high color value |
| CN112608620A (en) * | 2014-10-30 | 2021-04-06 | 三荣源有限公司 | Method for removing geniposide, genipin or both |
| CN114716841A (en) * | 2022-05-05 | 2022-07-08 | 安徽农业大学 | Preparation method of high-color-value gardenia yellow pigment |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112608620A (en) * | 2014-10-30 | 2021-04-06 | 三荣源有限公司 | Method for removing geniposide, genipin or both |
| CN108558645A (en) * | 2018-05-18 | 2018-09-21 | 武汉雅仕博科技有限公司 | The method that crocin is extracted from cape jasmine |
| CN108558645B (en) * | 2018-05-18 | 2021-04-09 | 武汉雅仕博科技有限公司 | Method for extracting crocin from gardenia |
| CN108774407A (en) * | 2018-05-30 | 2018-11-09 | 山东省农业科学院农产品研究所 | A kind of extracting method of gardenia yellow pigment with high color value |
| CN108774407B (en) * | 2018-05-30 | 2019-06-11 | 山东省农业科学院农产品研究所 | A kind of extracting method of gardenia yellow pigment with high color value |
| CN114716841A (en) * | 2022-05-05 | 2022-07-08 | 安徽农业大学 | Preparation method of high-color-value gardenia yellow pigment |
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