CN101165104B - Technique for preparing gardenia yellow pigment - Google Patents
Technique for preparing gardenia yellow pigment Download PDFInfo
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- CN101165104B CN101165104B CN200610137265A CN200610137265A CN101165104B CN 101165104 B CN101165104 B CN 101165104B CN 200610137265 A CN200610137265 A CN 200610137265A CN 200610137265 A CN200610137265 A CN 200610137265A CN 101165104 B CN101165104 B CN 101165104B
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Abstract
The process of preparing gardenia yellow pigment includes the following steps: 1. simultaneous water extracting and enzymolysis to obtain extracted solution; 2. adding calcium salt into the extractedsolution to clarify, centrifuging and ultrafiltering to obtain filtrate; and 3. macroporous resin adsorption of the filtrate, three-section eluting chromatography, concentrating, and drying to obtaingardenia yellow pigment with high color number and low jasminodin content. The process is simple and suitable for use in industrial production and can eliminate jasminodin chlorogenic acid effectively, and the gardenia yellow pigment product has A238/A440 not higher than 0.4, A325/A440 not higher than 0.35, color number of about 400 and stable quality.
Description
Technical field
The present invention relates to a kind of preparation technology's of natural food pigment, particularly Gardenia Yellow preparation technology.
Background technology
Gardenia Yellow is one of main component in the madder wort cape jasmine dry fruit, for using more a kind of water-soluble pigment at present, its main coloring components is Crocin (Crocin) and trans-crocetin (Crocetin), also contains compositions such as a small amount of iridoid glycoside, flavones, chlorogenic acid in addition.Gardenia Yellow is nontoxic, safe, certain nutrient value and nourishing function are arranged, also have good water solubility, strong coloring force, characteristics such as comparatively stable simultaneously, therefore be widely used in food colors such as beverage, cake, flour products, candy, drinks, milk-product, also can be used for the dyeing of silk, cotton, also can be used for makeup, medicine is painted and medicine material, feedstuff raw material.
Be to fade easily and " green change " phenomenon than distinct issues during Gardenia Yellow is used.Crocin and trans-crocetin are water-soluble carotenoid, contain a plurality of conjugated double bonds, and easy and electrophilic reagent generation addition reaction is damaged chromophoric group, and fades gradually.Problem generally can be resolved by adding sequestrant, antioxidant and regulating pH value hereto.And " green change " mainly is owing to the iridoid glycoside constituents hydrolysis under the effect of proteolytic enzyme or beta-glucosidase in the pigment, and hydrolysate and amino acids composition react, and the generation blue material causes.In addition, the chlorogenic acid in the pigment is oxidized easily, and makes painted food deepening.Therefore, the key of Gardenia Yellow preparation is to remove iridoid glycoside and the chlorogenic acid in the pigment.At present, it is generally acknowledged in the world the maximum absorbance (maximum absorption wavelength is 238nm) of jasminoidin (main component of iridoid glycosides in the cape jasmine) and the ratio (A of the maximum absorbance (maximum absorption wavelength is 440nm) of Crocin and trans-crocetin
238/ A
440) be controlled at below 0.4, can avoid the generation of " green change "; Simultaneously, for improving pigment stability, also require the maximum absorbance (maximum absorption wavelength is 325nm) of chlorogenic acid and the ratio (A of the maximum absorbance of Crocin and trans-crocetin
325/ A
440) should be controlled at below 0.35.
Known Gardenia Yellow production technique generally is with raw material pulverizing, with the extraction using alcohol about water extraction or 50%, after clarification, concentrating, utilizes the refining finished product that obtains of column chromatography (generally being macroporous resin).During extraction, because of containing impurity such as a large amount of pectin, carbohydrate and protein in the raw material, subsequent disposal bothers, and extraction time is long with water extraction, when refining, for reaching A
238/ A
440＜0.4, need secondary to cross post or employing organic solvent extraction usually, complex operation, cost is higher.
Summary of the invention
The invention provides a kind of Gardenia Yellow preparation method, this method technology is simple, and do not need secondary to cross post or use organic solvent extraction, the constant product quality that makes, and Gardenia Yellow look valency is about 400.
Technique for preparing gardenia yellow pigment of the present invention may further comprise the steps:
1, water extraction: will the cape jasmine dry fruit pulverize the back and add 10-15 water doubly, and add polygalacturonase, under temperature 45-50 ℃, the condition of pH value 3-5, extract 2-3 time, 1-2 hour at every turn, make extracting solution;
2, clarification: adding the calcium salt of 0.5-1% in extracting solution, left standstill after stirring 1-2 hour, behind disk centrifugal, is 5-10 ten thousand daltonian ultra-filtration membranes by the molecular weight that dams, and collects filtrate;
3, chromatography: with filtrate through absorption with macroporous adsorbent resin, successively with the concentration of the ethanol of the concentration 20-30% of the water of 4-6 times of resin volume, 4-6 times resin volume, 2-4 times resin volume greater than 40% ethanol elution, collect the elutriant of concentration after greater than 40% ethanol elution;
4, concentrate drying: concentrate drying: with the concentration of the collecting elutriant decompression recycling ethanol after greater than 40% ethanol elution, through concentrate, drying makes finished product.
The described cape jasmine dry fruit is pulverized is to be ground into the particle that diameter is 1-2mm.
Described polygalacturonase is 0.003% water weight, activity greater than 30,000 polygalacturonase.
Described calcium salt is calcium chloride, calcium sulfate etc.
The alcoholic acid optimum concn of concentration 20-30% is 25%, and concentration is 50% greater than 40% alcoholic acid optimum concn.
In the aforesaid step 4, behind the elutriant decompression recycling ethanol of concentration after greater than 40% ethanol elution, being concentrated into refractive power earlier is 10-25Brix (hundred sharp degree), carries out spraying drying or vacuum lyophilization again, can make the look valency about 400, A
238/ A
440≤ 0.4, A
325/ A
440≤ 0.35 Gardenia Yellow finished product.
In the aforesaid step 3, washing is in order to remove water-soluble impurities such as carbohydrate in the filtrate, protein, and chlorogenic acid, gardenoside are because polarity more also has the part can be by water elution simultaneously; The ethanol elution of concentration 20-30% is in order to remove chlorogenic acid, gardenoside more up hill and dale; Concentration is to be used for Gardenia Yellow is eluted greater than 40% ethanol.
The present invention compared with prior art has the following advantages:
1, when extracting, adds polygalacturonase and carry out enzymolysis, help to improve yield, and extracting solution is clarified more, reduce the subsequent disposal operation, make the more succinct smoothness of technology;
2, add calcium salt behind the enzymolysis and clarify, can reduce the content of protein and polyphenols in the extracting solution;
3, membrane technique and chromatographic technique are combined, improved the clarity of post feed liquid, can promote the adsorption efficiency of resin and prolong its work-ing life, help to reduce production costs and enhance productivity;
4, utilize stepwise elution, do not need secondary column chromatography or extraction, just can remove gardenoside and chlorogenic acid preferably, make the A of product
238/ A
440Value≤0.4, A
325/ A
440≤ 0.35, the look valency is about 400, and constant product quality, is suitable for large-scale industrialization production.
Embodiment
Embodiment one:
1. get cape jasmine dry fruit 1kg, be ground into the particle that diameter is 1-2mm, add 15 kg of water, add the polygalacturonase (activity＞30,000) of 0.45g again, regulate pH value to 4.5 with citric acid, 50 ℃ were extracted 1.5 hours down, extract united extraction liquid 2 times.
2. adding 150g calcium chloride in extracting solution, stir, placed 1 hour, behind disk centrifugal, is 100,000 daltonian ultra-filtration membranes by the molecular weight that dams, and obtains the filtrate of clear.
3. with behind the chromatography column of above-mentioned solution stream through the 1kg macroporous adsorbent resin is housed, use 50% the ethanol elution of 25% ethanol, the 6L of water, the 15L of 15L successively, flow rate control is at 4L/h, collects the elutriant behind 50% the ethanol elution.
4. the elutriant behind 50% the ethanol elution that will collect under 60 ℃, decompression recycling ethanol, and after being concentrated into refractive power and being 10Brix (hundred sharp degree), carry out spraying drying, obtaining 18g look valency is 386, A
238/ A
440Value is 0.39, A
325/ A
440Value is 0.34 Gardenia Yellow powder.
Embodiment two:
1. get cape jasmine dry fruit 1kg, be ground into the particle that diameter is 1-2mm, add 15 kg of water, add the polygalacturonase (activity＞30,000) of 0.45g again, regulate pH value to 4.5 with citric acid, 50 ℃ were extracted 1.5 hours down, extract united extraction liquid 2 times.
2. adding 150g calcium sulfate in extracting solution, stir, placed 1 hour, behind disk centrifugal, is 80,000 daltonian ultra-filtration membranes by the molecular weight that dams, and obtains the filtrate of clear.
3. with behind the chromatography column of above-mentioned solution stream through the 1kg macroporous adsorbent resin is housed, use 50% the ethanol elution of 25% ethanol, the 6L of water, the 15L of 15L successively, flow rate control is at 4L/h, collects the elutriant behind 50% the ethanol elution.
4. the elutriant behind 50% the ethanol elution that will collect under 60 ℃, decompression recycling ethanol, and after being concentrated into refractive power and being 10Brix (hundred sharp degree), carry out spraying drying, obtaining 15g look valency is 403, A
238/ A
440Value is 0.38, A
325/ A
440Value is 0.33 Gardenia Yellow powder.
Embodiment three:
1. get cape jasmine dry fruit 1kg, be ground into the particle that diameter is 1-2mm, add 15 kg of water, add the polygalacturonase (activity＞30,000) of 0.45g again, regulate pH value to 4.5 with citric acid, 50 ℃ were extracted 1.5 hours down, extract united extraction liquid 2 times.
Adding 150g calcium chloride in extracting solution, stir, place after 1 hour, behind disk centrifugal, is 50,000 daltonian ultra-filtration membranes by the molecular weight that dams, and obtains the filtrate of clear.
3. with behind the chromatography column of above-mentioned solution stream through the 1kg macroporous adsorbent resin is housed, use 50% the ethanol elution of 25% ethanol, the 6L of water, the 15L of 15L successively, flow rate control is at 4L/h, collects the elutriant behind 50% the ethanol elution.
4. the elutriant behind 50% the ethanol elution that will collect under 60 ℃, decompression recycling ethanol, and after being concentrated into refractive power and being 15Brix (hundred sharp degree), carry out spraying drying, obtaining 16g look valency is 396, A
238/ A
440Value is 0.38, A
325/ A
440Value is 0.32 Gardenia Yellow powder.
Claims (6)
1. technique for preparing gardenia yellow pigment is characterized in that: may further comprise the steps:
(1) water extraction: will the cape jasmine dry fruit pulverize the back and add 10-15 water doubly, and add polygalacturonase, under temperature 45-50 ℃, the condition of pH value 3-5, extract 2-3 time, 1-2 hour at every turn, make extracting solution;
(2) clarification: adding calcium sulfate, the calcium chloride of 0.5-1% in extracting solution, left standstill after stirring 1-2 hour, behind disk centrifugal, is 5-10 ten thousand daltonian ultra-filtration membranes by the molecular weight that dams, and collects filtrate;
(3) chromatography: with filtrate through absorption with macroporous adsorbent resin, successively with the concentration of the ethanol of the concentration 20-30% of the water of 4-6 times of resin volume, 4-6 times resin volume, 2-4 times resin volume greater than 40% ethanol elution, collect the elutriant of concentration after greater than 40% ethanol elution;
(4) concentrate drying: with the concentration of the collecting elutriant decompression recycling ethanol after greater than 40% ethanol elution, through concentrate, drying makes finished product.
2. according to the described technique for preparing gardenia yellow pigment of claim 1, it is characterized in that: described the cape jasmine dry fruit is pulverized to being ground into the particle of diameter for-2mm.
3. according to the described technique for preparing gardenia yellow pigment of claim 1, it is characterized in that: described polygalacturonase is 0.003% water weight, activity greater than 30,000 polygalacturonase.
4. according to the described technique for preparing gardenia yellow pigment of claim 1, it is characterized in that: it is 10-25Brix (hundred sharp degree) that described simmer down to is concentrated into refractive power.
5. according to the described technique for preparing gardenia yellow pigment of claim 1, it is characterized in that: described concentration is that the alcohol concn of 20-30% is 25%, and described concentration is 50% greater than 40% concentration of ethanol.
6. according to the described technique for preparing gardenia yellow pigment of claim 1, it is characterized in that: described dry spraying drying or the vacuum lyophilization of adopting.
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|---|---|---|---|
| CN200610137265A CN101165104B (en) | 2006-10-18 | 2006-10-18 | Technique for preparing gardenia yellow pigment |
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|---|---|---|---|
| CN200610137265A CN101165104B (en) | 2006-10-18 | 2006-10-18 | Technique for preparing gardenia yellow pigment |
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| CN101165104A CN101165104A (en) | 2008-04-23 |
| CN101165104B true CN101165104B (en) | 2010-05-12 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107949370A (en) * | 2015-09-09 | 2018-04-20 | 皮埃尔法布雷医药公司 | For making the capejasmine extract of pigmenting of skin |
Families Citing this family (16)
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|---|---|---|---|---|
| CN101411466B (en) * | 2008-11-24 | 2012-08-08 | 浙江省中药研究所有限公司 | Method for preparing cape jasmine yellow pigment using cape jasmine as raw material |
| CN101863754A (en) * | 2009-04-17 | 2010-10-20 | 杭州法和医药科技有限公司 | Preparation method of crocetin, gardenia yellow pigment and saffron pigment |
| CN101659794B (en) * | 2009-09-27 | 2012-08-29 | 广西山云生化科技有限公司 | New process for extracting high-purity gardenia yellow pigment by membrane separation and purification technology |
| CN101824232B (en) * | 2010-05-31 | 2012-12-05 | 福建农林大学 | Preparation method of gardenia green pigment |
| CN102344692B (en) * | 2011-08-10 | 2013-11-13 | 浙江工业大学 | Method for extracting gardenia yellow pigment from gardeniae longicarpae fruit |
| CN103060078A (en) * | 2011-10-20 | 2013-04-24 | 中国科学院兰州化学物理研究所 | Method for aqueous enzymatic extraction of gardenia oil |
| CN103060077A (en) * | 2011-10-20 | 2013-04-24 | 中国科学院兰州化学物理研究所 | Method for preparation of gardenia oil, gardenia green pigment and gardenia blue pigment through synchronous reaction |
| CN102585545A (en) * | 2011-12-29 | 2012-07-18 | 浙江惠松制药有限公司 | Preparation method for water gardenia flavochrome |
| CN102816455A (en) * | 2012-08-06 | 2012-12-12 | 集美大学 | Method for extracting pigment and pectin from pineapple peels |
| CN102911513B (en) * | 2012-08-17 | 2014-03-12 | 江苏久吾高科技股份有限公司 | Extraction method of gardenia yellow pigment |
| CN103735633B (en) * | 2013-12-30 | 2016-01-20 | 南京博士牛生物科技有限公司 | A kind of preparation method of instant gardenia powder |
| CN103740130B (en) * | 2014-01-11 | 2015-09-23 | 云南瑞宝生物科技有限公司 | A kind of preparation method of Gardenia Yellow |
| CN104382015B (en) * | 2014-10-31 | 2016-03-30 | 朱彩凤 | A kind of preparation method of gardenia oral liquid |
| CN108912732A (en) * | 2018-08-10 | 2018-11-30 | 湖北康乐源生物科技有限公司 | A method of high-purity gardenia yellow pigment is extracted with cape jasmine fresh fruit |
| CN108992542A (en) * | 2018-08-20 | 2018-12-14 | 江苏恒瑞泽朗生物工程有限公司 | A kind of plant extraction process |
| CN111675923B (en) * | 2020-06-24 | 2021-05-25 | 河南大农联生物工程有限公司 | Method for extracting gardenia pigment through steam explosion and application method of extracted pigment |
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| CN1151420A (en) * | 1995-11-30 | 1997-06-11 | 湖南省林业科学研究所 | Jasmin uranidin prodn. tech. |
| CN1544532A (en) * | 2003-11-25 | 2004-11-10 | 中国科学院武汉植物研究所 | Method for preparing gardenia yellow pigment |
| CN1807441A (en) * | 2006-02-23 | 2006-07-26 | 江南大学 | Method for producing high purity jasminoidin and high color number gardenia yellow pigment |
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2006
- 2006-10-18 CN CN200610137265A patent/CN101165104B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1151420A (en) * | 1995-11-30 | 1997-06-11 | 湖南省林业科学研究所 | Jasmin uranidin prodn. tech. |
| CN1544532A (en) * | 2003-11-25 | 2004-11-10 | 中国科学院武汉植物研究所 | Method for preparing gardenia yellow pigment |
| CN1807441A (en) * | 2006-02-23 | 2006-07-26 | 江南大学 | Method for producing high purity jasminoidin and high color number gardenia yellow pigment |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107949370A (en) * | 2015-09-09 | 2018-04-20 | 皮埃尔法布雷医药公司 | For making the capejasmine extract of pigmenting of skin |
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| CN101165104A (en) | 2008-04-23 |
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