CN108841892A - The method of Production by Enzymes gardenia red pigment - Google Patents
The method of Production by Enzymes gardenia red pigment Download PDFInfo
- Publication number
- CN108841892A CN108841892A CN201810909459.1A CN201810909459A CN108841892A CN 108841892 A CN108841892 A CN 108841892A CN 201810909459 A CN201810909459 A CN 201810909459A CN 108841892 A CN108841892 A CN 108841892A
- Authority
- CN
- China
- Prior art keywords
- gardenia red
- gardenoside
- aqueous solution
- esterification
- red pigment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000001054 red pigment Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 36
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 28
- 102000004190 Enzymes Human genes 0.000 title claims abstract description 22
- 108090000790 Enzymes Proteins 0.000 title claims abstract description 22
- 240000001972 Gardenia jasminoides Species 0.000 title description 2
- 241000157835 Gardenia Species 0.000 claims abstract description 79
- XJMPAUZQVRGFRE-SCHFUKFYSA-N Gardenoside Natural products O=C(OC)C=1[C@H]2[C@H]([C@H](O[C@H]3[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O3)OC=1)[C@@](O)(CO)C=C2 XJMPAUZQVRGFRE-SCHFUKFYSA-N 0.000 claims abstract description 74
- XJMPAUZQVRGFRE-AYDWLWLASA-N methyl (1s,4as,7s,7as)-7-hydroxy-7-(hydroxymethyl)-1-[(2s,3r,4s,5s,6r)-3,4,5-trihydroxy-6-(hydroxymethyl)oxan-2-yl]oxy-4a,7a-dihydro-1h-cyclopenta[c]pyran-4-carboxylate Chemical compound O([C@@H]1OC=C([C@@H]2[C@H]1[C@](C=C2)(O)CO)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O XJMPAUZQVRGFRE-AYDWLWLASA-N 0.000 claims abstract description 74
- 239000007864 aqueous solution Substances 0.000 claims abstract description 68
- 230000032050 esterification Effects 0.000 claims abstract description 51
- 238000005886 esterification reaction Methods 0.000 claims abstract description 51
- 239000000287 crude extract Substances 0.000 claims abstract description 19
- 229930182470 glycoside Natural products 0.000 claims abstract description 11
- 150000002338 glycosides Chemical class 0.000 claims abstract description 10
- QNAYBMKLOCPYGJ-REOHCLBHSA-N L-alanine Chemical compound C[C@H](N)C(O)=O QNAYBMKLOCPYGJ-REOHCLBHSA-N 0.000 claims abstract description 9
- 235000004279 alanine Nutrition 0.000 claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 36
- 235000018958 Gardenia augusta Nutrition 0.000 claims description 28
- 244000111489 Gardenia augusta Species 0.000 claims description 27
- 239000011347 resin Substances 0.000 claims description 27
- 229920005989 resin Polymers 0.000 claims description 27
- 238000001179 sorption measurement Methods 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 19
- 239000003480 eluent Substances 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 16
- 238000000605 extraction Methods 0.000 claims description 13
- 239000007788 liquid Substances 0.000 claims description 13
- 238000001914 filtration Methods 0.000 claims description 12
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 claims description 11
- 239000012141 concentrate Substances 0.000 claims description 10
- 239000012530 fluid Substances 0.000 claims description 10
- 238000010828 elution Methods 0.000 claims description 9
- 235000013399 edible fruits Nutrition 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 8
- 238000001694 spray drying Methods 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 6
- 238000007789 sealing Methods 0.000 claims description 6
- 229930182478 glucoside Natural products 0.000 claims description 4
- 150000008131 glucosides Chemical class 0.000 claims description 4
- 238000007670 refining Methods 0.000 claims description 4
- 108010076282 Factor IX Proteins 0.000 claims description 2
- 238000010936 aqueous wash Methods 0.000 claims 1
- 230000007071 enzymatic hydrolysis Effects 0.000 abstract description 6
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 abstract description 6
- 238000004176 ammonification Methods 0.000 abstract description 4
- 239000002994 raw material Substances 0.000 abstract description 3
- 238000009776 industrial production Methods 0.000 abstract description 2
- 238000001035 drying Methods 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 description 14
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 12
- 239000000243 solution Substances 0.000 description 11
- 230000008569 process Effects 0.000 description 10
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 9
- 238000010521 absorption reaction Methods 0.000 description 7
- 235000019441 ethanol Nutrition 0.000 description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 5
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000001976 enzyme digestion Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 3
- 239000003814 drug Substances 0.000 description 3
- 150000002148 esters Chemical class 0.000 description 3
- 239000006004 Quartz sand Substances 0.000 description 2
- 244000061458 Solanum melongena Species 0.000 description 2
- 239000002250 absorbent Substances 0.000 description 2
- 230000002745 absorbent Effects 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 229910021529 ammonia Inorganic materials 0.000 description 2
- 239000004281 calcium formate Substances 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000001514 detection method Methods 0.000 description 2
- 229940079593 drug Drugs 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000000855 fermentation Methods 0.000 description 2
- 230000004151 fermentation Effects 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000011068 loading method Methods 0.000 description 2
- 239000000395 magnesium oxide Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 239000000758 substrate Substances 0.000 description 2
- SEBIKDIMAPSUBY-ARYZWOCPSA-N Crocin Chemical compound C([C@H]1O[C@H]([C@@H]([C@@H](O)[C@@H]1O)O)OC(=O)C(C)=CC=CC(C)=C\C=C\C=C(/C)\C=C\C=C(C)C(=O)O[C@H]1[C@@H]([C@@H](O)[C@H](O)[C@@H](CO[C@H]2[C@@H]([C@@H](O)[C@H](O)[C@@H](CO)O2)O)O1)O)O[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O SEBIKDIMAPSUBY-ARYZWOCPSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- IBFYXTRXDNAPMM-BVTMAQQCSA-N Geniposide Chemical compound O([C@@H]1OC=C([C@@H]2[C@H]1C(=CC2)CO)C(=O)OC)[C@@H]1O[C@H](CO)[C@@H](O)[C@H](O)[C@H]1O IBFYXTRXDNAPMM-BVTMAQQCSA-N 0.000 description 1
- IBFYXTRXDNAPMM-FZEIBHLUSA-N Geniposide Natural products COC(=O)C1=CO[C@@H](O[C@H]2O[C@@H](CO)[C@H](O)[C@@H](O)[C@@H]2O)[C@H]2[C@@H]1CC=C2CO IBFYXTRXDNAPMM-FZEIBHLUSA-N 0.000 description 1
- 241000123069 Ocyurus chrysurus Species 0.000 description 1
- VGLLGNISLBPZNL-RBUKDIBWSA-N arborescoside Natural products O=C(OC)C=1[C@@H]2C([C@H](O[C@H]3[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O3)OC=1)=C(CO)CC2 VGLLGNISLBPZNL-RBUKDIBWSA-N 0.000 description 1
- 230000001580 bacterial effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000008280 blood Substances 0.000 description 1
- 210000004369 blood Anatomy 0.000 description 1
- 235000021466 carotenoid Nutrition 0.000 description 1
- 150000001747 carotenoids Chemical class 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
- 238000004040 coloring Methods 0.000 description 1
- 239000009627 gardenia yellow Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 239000003595 mist Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 230000005180 public health Effects 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000012429 reaction media Substances 0.000 description 1
- 238000009287 sand filtration Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P17/00—Preparation of heterocyclic carbon compounds with only O, N, S, Se or Te as ring hetero atoms
- C12P17/10—Nitrogen as only ring hetero atom
- C12P17/12—Nitrogen as only ring hetero atom containing a six-membered hetero ring
Landscapes
- Organic Chemistry (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Microbiology (AREA)
- General Chemical & Material Sciences (AREA)
- Biotechnology (AREA)
- Health & Medical Sciences (AREA)
- Biochemistry (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- General Health & Medical Sciences (AREA)
- Genetics & Genomics (AREA)
- Preparation Of Compounds By Using Micro-Organisms (AREA)
Abstract
The present invention provides the methods of Production by Enzymes gardenia red pigment, belong to gardenia red pigment preparation technical field, this approach includes the following steps：1) Gardenoside aqueous solution is taken, 80~90 DEG C of 26~39h of esterification obtain esterification Gardenoside aqueous solution；2) the glycosides valence E of esterification Gardenoside aqueous solution is adjusted238It is 4~5 for 10~15, pH, then the esterification Gardenoside aqueous solution after adjusting is mixed with glucuroide, alanine, 43~48 DEG C of 6~7d of enzymatic hydrolysis obtains gardenia red crude extract；3) gardenia red crude extract purified, be concentrated, drying acquisition gardenia red pigment.The present invention obtains gardenia red crude extract after reacting by esterification and enzymatic hydrolysis ammonification using Gardenoside as raw material, then gardenia red crude extract is purified, be concentrated, dries acquisition gardenia red pigment.The gardenia red pigment tone glow that method of the invention is extracted is stablized, and pure color valence is high, and production cost is low, is conducive to large-scale industrial production.
Description
Technical field
The present invention relates to gardenia red pigment preparation technical field more particularly to the methods of Production by Enzymes gardenia red pigment.
Background technique
Madder wort cape jasmine is a kind of dual-purpose of drug and food traditional Chinese medicine, has clearing heat and removing internal heat, removing pattogenic heat from the blood and toxic material from the body effect, 1998
What year Ministry of Public Health announced is both food again in the kind list of drug, and cape jasmine is first, and gardenia red pigment is that one kind is water-soluble
Property carotenoid, be it is a kind of integrate coloring multifunctional health natural plant pigment.
CN103265824B provides the production and refining methd of a kind of gardenia red pigment in the prior art, but this method needs
Strain fermentation is wanted, course of fermentation and fermented product quality are limited by bacterial activity, are unfavorable for large-scale promotion；
CN102174608A provides a kind of method for extracting gardenia red pigment, and this method is to have adsorbed the resin of geniposide as reaction
Medium increases reaction cost to the more demanding of production equipment.In consideration of it, lacking at this stage, a kind of production cost is low, product
The method of good, conducive to large-scale promotion the production gardenia red pigment of quality.
Summary of the invention
The purpose of the present invention is to provide a kind of method of Production by Enzymes gardenia red pigment, this method is at low cost, it is big to be conducive to
The gardenia red pigment that scale is promoted and extraction obtains is high-quality.
In order to achieve the above-mentioned object of the invention, the present invention provides following technical scheme：
The present invention provides a kind of methods of Production by Enzymes gardenia red pigment, include the following steps：
1) Gardenoside aqueous solution is obtained into esterification Gardenoside aqueous solution in 80~90 DEG C of 26~39h of esterification；
2) the glycosides valence E of the esterification Gardenoside aqueous solution is adjusted238It is 4~5 for 10~15, pH, then by the esterification after adjusting
Gardenoside aqueous solution is mixed with glucuroide, alanine, and 43~48 DEG C of sealings digest 6~7d, obtains gardenia red crude extract；
3) the gardenia red crude extract purified, be concentrated, dry acquisition gardenia red pigment；
The glucoside valence E of Gardenoside aqueous solution in the step 1)238It is 20~25；The pH value of the Gardenoside aqueous solution is 10
~12；
The mass ratio of esterification Gardenoside aqueous solution and glucuroide after adjusting in the step 2) is 200~300：1,
The mass ratio of esterification Gardenoside aqueous solution and alanine after adjusting is 35~45：1.
Preferably, the preparation method of the Gardenoside aqueous solution includes the following steps：
A) by cape jasmine dry powder with pure water soak extraction 7~8 times, filtered fluid is obtained by filtration after combined extract；
B) filtered fluid obtained in step a) is successively purified through macroporous resin adsorption, pure water removal of impurities and ethanol water
Elution, obtains eluent；
C) eluent in step b) is obtained into Gardenoside aqueous solution through vacuum-concentrcted.
Preferably, the cape jasmine dry powder partial size is 8~12mm.
Preferably, the time of each soak extraction of cape jasmine dry powder is 1~3h in the step a).
Preferably, macroreticular resin is LX-1 macroreticular resin in the step b).
Preferably, the cocnentration factor 9~11 being concentrated in the step 3)：1.
Preferably, the purifying in the step 3) includes the following steps：It will successively be adopted after gardenia red crude extract filtering
Purified with macroporous resin adsorption, obtain gardenia red refining liquid after pure water removal of impurities and ethanol water elution；The ethyl alcohol is water-soluble
The volumn concentration of liquid is 75%~80%；The macroreticular resin is LX-1 macroreticular resin.
Preferably, concentration is vacuum-concentrcted in the step 3), the E530 of obtained gardenia red concentrate is 9~
12。
Preferably, dry in the step 3) is centrifugal spray drying.
Beneficial effects of the present invention：The present invention provides a kind of methods of Production by Enzymes gardenia red pigment, and this method is with Cape jasmine
Sub- glycosides is raw material, by obtaining gardenia red crude extract after esterification and enzymatic hydrolysis ammonification reaction, then by gardenia red crude extract into
Row purifying, concentration, dry acquisition gardenia red pigment.The gardenia red pigment tone glow that method of the invention is extracted is stablized,
Pure color valence is up to 60 (E1%1cm) or more, and this method production cost is low, is conducive to large-scale industrial production.
Specific embodiment
The present invention provides a kind of methods of Production by Enzymes gardenia red pigment, include the following steps：
1) Gardenoside aqueous solution is obtained into esterification Gardenoside aqueous solution in 80~90 DEG C of 26~39h of esterification；
2) the glycosides valence E of the esterification Gardenoside aqueous solution is adjusted238It is 4~5 for 10~15, pH, then by the esterification after adjusting
Gardenoside aqueous solution is mixed with glucuroide, alanine, and 43~48 DEG C of sealings digest 6~7d, obtains gardenia red crude extract；
3) the gardenia red crude extract purified, be concentrated, dry acquisition gardenia red pigment；
The glucoside valence E of Gardenoside aqueous solution in the step 1)238It is 20~25；The pH value of the Gardenoside aqueous solution is 10
~12；
The mass ratio of esterification Gardenoside aqueous solution and glucuroide after adjusting in the step 2) is 200~300：1,
The mass ratio of esterification Gardenoside aqueous solution and alanine after adjusting is 35~45：1.
In the present invention, the raw material for extracting gardenia red pigment is Gardenoside；In specific implementation process of the invention,
The Gardenoside is extracted from cape jasmine dry powder and is obtained；The cape jasmine dry powder partial size is 8~12mm, preferably 10mm.
In specific implementation process of the invention, cape jasmine dry fruit is crushed, obtains cape jasmine dry powder；The cape jasmine dry fruit comes
Derived from commercially available；The place of production of the cape jasmine dry fruit is preferably Hubei, Jiangxi, Guangxi；The long fruit of the cape jasmine dry fruit is preferably 4cm；
The diameter of the cape jasmine dry fruit is preferably 2cm；The equipment of the pulverization process is preferably Universalpulverizer；The Universalpulverizer
Preferably 400 type toothed disc type Universalpulverizers；The 400 type toothed disc type Universalpulverizer is purchased from Jianyang of Sichuan west of a city Seiko machine
Tool.
In the present invention, the extracting method of the Gardenoside preferably includes following steps：A) by cape jasmine dry powder with pure
Water soak extraction 7~8 times, the extracting solution after filtering merges after combined extract obtains filtered fluid；It b) will be obtained in step a)
Filtered fluid is purified through macroporous resin adsorption, obtains efflux；C) by the efflux in step b) through being concentrated under reduced pressure to give Gardenoside
Aqueous solution.
In the present invention, by cape jasmine dry powder with pure water soak extraction 7~8 times, filtering is obtained by filtration after combined extract
Liquid；The time of each soak extraction of cape jasmine dry powder is 1~3h；The cape jasmine dry powder of each soak extraction with it is pure
The mass ratio of water is 2:1~1:2, preferably 1:1；The method of the filtering is to be filtered using quartz sand.
After the present invention obtains filtered fluid, filtered fluid is successively purified through macroporous resin adsorption, pure water removal of impurities and ethanol water
Solution elution, obtains eluent；The macroreticular resin is LX-1 macroreticular resin；The flow velocity of the adsorption liquid is preferably 10~
15mL/min, more preferably 12~13mL/min.
Pure water is added into adsorption column in pure water dedoping step by the present invention, cleans；The use of the pure water
Amount is preferably 4~5BV, more preferably 4.5BV；The flow velocity of the pure water is preferably 10~15mL/min, more preferably 12~
13mL/min。
The eluent that the present invention uses during ethanol elution is ethanol water；The water-soluble volume hundred of the ethyl alcohol
Dividing content is 70%~80%, preferably 75%；The dosage of the ethanol water is preferably 2BV；The flow velocity of the eluent
Preferably 0.3~0.5BV/h, more preferably 0.4BV/h.
The present invention obtains gardenia red concentrate after obtaining eluent, by eluent is concentrated；In the present invention, described dense
Contracting is preferably vacuum-concentrcted；The pressure of the vacuum-concentrcted is preferably -0.08~-0.09MPa, more preferably -
0.085MPa；The cocnentration factor of the vacuum-concentrcted is preferably 9~11：1, more preferably 10：1.
In specific implementation process of the invention, the UV-vis absorption curve of tracing detection adsorption column efflux works as elution
When Gardenoside absorption peak occurs at 238nm in liquid, picking up eluent, Gardenia Yellow is adsorbed at this time；When eluent tone shoals Huang
When, stopping picks up eluent.
The present invention takes Gardenoside aqueous solution after obtaining Gardenoside aqueous solution, and 80~90 DEG C of 26~39h of esterification obtain ester
Change Gardenoside aqueous solution；The temperature of the esterification is preferably 85 DEG C；The time of the esterification is preferably 30~35h；The cape jasmine
The glucoside valence E of glycosides aqueous solution238It is 20~25, preferably 21~24, more preferably 22~23；The pH value of the Gardenoside aqueous solution
It is 10~12, preferably 11；The reagent for adjusting Gardenoside aqueous solution glycosides valence is preferably pure water；The adjusting Gardenoside water
The reagent of pH value of solution is preferably NaOH aqueous solution；The mass percentage of the NaOH aqueous solution is preferably 20%；The esterification
The mode heated in treatment process is preferably steam jacket heating.
Gardenoside aqueous solution is placed in steam jacket in the specific implementation process and carries out the first esterification treatment by the present invention, is obtained
Primary esterification Gardenoside aqueous solution；The temperature of first esterification treatment is preferably 80~90 DEG C, and more preferably 85 DEG C；Described
The time of one esterification treatment is preferably 2~3h.The present invention stops heating, preliminary ester after obtaining primary esterification cape jasmine water glycosides solution
Change Gardenoside aqueous solution and stand the second esterification of progress in steam jacket, obtains esterification Gardenoside aqueous solution；The standing when
Between preferably 24~36h, more preferably 30h；The temperature of the standing is preferably 80~90 DEG C, and more preferably 85 DEG C.
The present invention adjusts the glycosides valence E of esterification Gardenoside aqueous solution after obtaining esterification Gardenoside aqueous solution238It is 10~15,
PH is 4~5, then the esterification Gardenoside aqueous solution after adjusting is mixed with glucuroide, alanine, 43~48 DEG C of enzymatic hydrolysis 6~
7d obtains gardenia red crude extract；The reagent for adjusting esterification Gardenoside aqueous solution glycosides valence is preferably pure water；The adjusting ester
The reagent for changing Gardenoside aqueous solution pH is preferably food-grade Citric acid crystal；Esterification Gardenoside aqueous solution and Portugal after the adjusting
The ratio of polyglycoside enzyme is 200~300：1, preferably 250：1；Esterification Gardenoside aqueous solution and alanine after the adjusting
Ratio is 35~45：1, preferably 40：1；Enzyme digestion reaction sealing carries out in the step 2)；The time of the enzyme digestion reaction is preferred
For 6.5d；The temperature of the enzyme digestion reaction is preferably 45 DEG C；The mode of the enzyme digestion reaction heating is preferably hot water jacket's heating.
The present invention after obtaining gardenia red crude extract, will gardenia red crude extract filtering after using macroporous resin adsorption purifying,
Gardenia red refining liquid is obtained after pure water removal of impurities and ethanol water elution；The filter type is preferably diatomite and/or filter
Bag, more preferably diatomite filter.
In specific implementation process of the invention, gardenia red crude extract is successively purified with macroporous resin adsorption, pure water
Removal of impurities, ethanol water elution, obtains gardenia red extract；The macroreticular resin is preferably LX-1 macroreticular resin；The purifying
The adsorption liquid that process uses is preferably gardenia red crude extract after diatomite filtering；The flow velocity of the adsorption liquid is preferably 1BV/h.This
Invention is in pure water dedoping step, and the dosage of the pure water is preferably 4~5BV, more preferably 4.5BV.The present invention is in second
In alcohol solution elution process, the volumn concentration of the ethanol water is 75%~80%；The ethanol water
Dosage is preferably 1~3BV, more preferably 2BV；The flow velocity of the eluent is preferably 0.5BV/h.
The present invention is after obtaining gardenia red extract, by gardenia red extract through being concentrated under reduced pressure into E530It is 9~12, stops
Concentration, obtains gardenia red concentrate；The pressure of the vacuum-concentrcted is preferably -0.08~-0.09MPa, more preferably -
0.085MPa；The cocnentration factor of the vacuum-concentrcted is 9~11：1, more preferably 10:1.
For the present invention after obtaining gardenia red concentrate, gardenia red concentrate obtains gardenia red pigment through centrifugal spray drying；
The water content of the gardenia red pigment is preferably 3%~7%, and more preferably 5%.
In specific implementation process of the invention, after obtaining gardenia red concentrate, gardenia red concentrate is sprayed through centrifugation
Mist is dry to get gardenia red powder.
It is described in detail below with reference to method of the embodiment to Production by Enzymes gardenia red pigment provided by the invention, but
It is that they cannot be interpreted as limiting the scope of the present invention.
A kind of preparation method of the Gardenoside aqueous solution of embodiment 1
1) it extracts：It is 10mm that cape jasmine dry fruit, which is smashed with Universalpulverizer to material size diameter, obtains cape jasmine dry powder, will
For cape jasmine dry powder with pure water soak extraction 7 times, the cape jasmine dry powder of each soak extraction is 500g, each soak extraction it is pure
Water purification is 1000g, and each soak extraction 2h obtains filtered fluid after clarifying soak with quartz sand filtration.
2) macroporous resin purification：By above-mentioned filtered fluid LX-1 macroporous resin adsorption, control absorption column flow rate is 1BV/h.
The UV-vis absorption curve of tracing detection adsorption column adsorption liquid is picked up when Gardenoside absorption peak occurs at 238nm in adsorption liquid
Adsorption liquid gardenoside, when adsorption column efflux tone shoals Huang, stopping picks up efflux.
3) it is concentrated：The adsorption liquid vacuum-concentrcted that will be picked up, cocnentration factor 10：1, obtain Gardenoside aqueous solution.
A kind of method of the Production by Enzymes gardenia red pigment of embodiment 2
1) using the Gardenoside aqueous solution being prepared in embodiment 1 as reaction substrate.
2) esterification treatment：Gardenoside aqueous solution 1000g is taken, adjusts Gardenoside aqueous solution E with pure water238=20, use quality
It is 10 that the NaOH that volume basis amount is 20%, which adjusts Gardenoside solution ph, and the Gardenoside aqueous solution after above-mentioned adjusting is placed in heat
In 85 DEG C of progress 30h esterifications in water leg, esterification Gardenoside aqueous solution is obtained.
3) enzymatic hydrolysis ammonification reaction：Will esterification Gardenoside aqueous solution be placed in hot water jacket, and to esterification Gardenoside aqueous solution
Middle addition pure water adjusts E238=15, Citric acid crystal powder tune PH to 4.5 is added, adds the third ammonia of 6g glucuroide and 40g
Acid is heated to 45 DEG C of sealing thermal insulations and is digested for 7 days, stops when reaction solution tone is constant in peak value at aubergine and 530nm
Reaction, surveys E1% through UVPC530=2.6.
4) macroporous resin purification：It, will be anti-using a pillar equipped with the 500g macroporous absorbent resin LX-1 pre-processed
Gardenia red that should be good is through filtering loading absorption, and coutroi velocity 10mL/min is cleaned with 5000g/ column pure water, volumn concentration
It is eluted for 75% ethanol solution, obtains eluent.
5) it filters, be concentrated：It is 300g that eluent, which is filtered, is concentrated under reduced pressure into weight, and UVPC detects E1%530=10.5,
Detecting pure color valence is 65.6.
6) centrifugal spray drying：Gardenia red concentrate is through centrifugal spray drying up to gardenia red pigment.
A kind of method of the Production by Enzymes gardenia red pigment of embodiment 3
1) using the Gardenoside aqueous solution being prepared in embodiment 1 as reaction substrate.
2) esterification treatment：Gardenoside aqueous solution 2000g is taken, adjusts Gardenoside aqueous solution E with pure water238=20, use quality
It is 12 that the NaOH that volume basis amount is 20%, which adjusts Gardenoside solution ph, and the Gardenoside aqueous solution after above-mentioned adjusting is placed in heat
In 85 DEG C of progress 36h esterifications in water leg, esterification Gardenoside aqueous solution is obtained.
3) enzymatic hydrolysis ammonification reaction：Will esterification Gardenoside aqueous solution be placed in hot water jacket, and to esterification Gardenoside aqueous solution
Middle addition pure water adjusts E238=15, Citric acid crystal powder tune PH to 4.5 is added, adds the third ammonia of 12g glucuroide and 90g
Acid is heated to 45 DEG C of sealing thermal insulations and is digested for 8 days, stops when reaction solution tone is constant in peak value at aubergine and 530nm
Reaction, surveys E1% through UVPC530=2.85.
4) macroporous resin purification：It, will be anti-using two pillars equipped with the 500g macroporous absorbent resin LX-1 pre-processed
Gardenia red that should be good is through filtering loading absorption, and coutroi velocity 15mL/min is cleaned with 5000g/ column pure water, volumn concentration
It is eluted for 75% ethanol solution, obtains eluent.
5) it filters, be concentrated：It is 600g that eluent, which is filtered, is concentrated under reduced pressure into weight, and UVPC detects E1%530=11.6, inspection
Surveying pure color valence is 63.8.
6) centrifugal spray drying：Gardenia red concentrate is through centrifugal spray drying up to gardenia red pigment.
As seen from the above embodiment, the present invention provides the method for Production by Enzymes gardenia red pigment, this method is prepared
Gardenia red pigment pure color valence up to 60 (E1%1cm) or more, it is seen then that method of the invention has reached good technical effect.
The above is only a preferred embodiment of the present invention, it is noted that for the ordinary skill people of the art
For member, various improvements and modifications may be made without departing from the principle of the present invention, these improvements and modifications are also answered
It is considered as protection scope of the present invention.
Claims (9)
1. the method for Production by Enzymes gardenia red pigment, includes the following steps：
1) Gardenoside aqueous solution is obtained into esterification Gardenoside aqueous solution in 80~90 DEG C of 26~39h of esterification；
2) the glycosides valence E of the esterification Gardenoside aqueous solution is adjusted238It is 4~5 for 10~15, pH, then by the esterification cape jasmine after adjusting
Glycosides aqueous solution is mixed with glucuroide, alanine, and 43~48 DEG C of sealings digest 6~7d, obtains gardenia red crude extract；
3) the gardenia red crude extract purified, be concentrated, dry acquisition gardenia red pigment；
The glucoside valence E of Gardenoside aqueous solution in the step 1)238It is 20~25；The pH value of the Gardenoside aqueous solution is 10~12；
The mass ratio of esterification Gardenoside aqueous solution and glucuroide after adjusting in the step 2) is 200~300：1, it adjusts
The mass ratio of esterification Gardenoside aqueous solution and alanine afterwards is 35~45：1.
2. the method for Production by Enzymes gardenia red pigment according to claim 1, which is characterized in that the Gardenoside aqueous solution
Preparation method include the following steps：
A) by cape jasmine dry powder with pure water soak extraction 7~8 times, filtered fluid is obtained by filtration after combined extract；
B) filtered fluid obtained in step a) is successively purified through macroporous resin adsorption, pure water removal of impurities and ethanol aqueous wash
It is de-, obtain eluent；
C) eluent in step b) is obtained into Gardenoside aqueous solution through vacuum-concentrcted.
3. the method for Production by Enzymes gardenia red pigment according to claim 2, which is characterized in that the cape jasmine dry fruit powder
Diameter is 8~12mm.
4. the method for Production by Enzymes gardenia red pigment according to claim 3, which is characterized in that cape jasmine in the step a)
The time of each soak extraction of dry powder is 1~3h.
5. the method for Production by Enzymes gardenia red pigment according to claim 1, which is characterized in that macropore in the step b)
Resin is LX-1 macroreticular resin.
6. the method for Production by Enzymes gardenia red pigment according to claim 1, which is characterized in that concentration in the step 3)
Cocnentration factor 9~11：1.
7. the method for the Production by Enzymes gardenia red pigment according to claim 1, which is characterized in that in the step 3)
Purifying include the following steps：It will successively be removed using macroporous resin adsorption purifying, pure water after gardenia red crude extract filtering
Gardenia red refining liquid is obtained after the elution of miscellaneous and ethanol water；
The volumn concentration of the ethanol water is 75%~80%；
The macroreticular resin is LX-1 macroreticular resin.
8. the method for Production by Enzymes gardenia red pigment according to claim 1, which is characterized in that concentration in the step 3)
For vacuum-concentrcted, the E of obtained gardenia red concentrate530It is 9~12.
9. the method for Production by Enzymes gardenia red pigment according to claim 1, which is characterized in that dry in the step 3)
For centrifugal spray drying.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810909459.1A CN108841892A (en) | 2018-08-10 | 2018-08-10 | The method of Production by Enzymes gardenia red pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201810909459.1A CN108841892A (en) | 2018-08-10 | 2018-08-10 | The method of Production by Enzymes gardenia red pigment |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN108841892A true CN108841892A (en) | 2018-11-20 |
Family
ID=64193053
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201810909459.1A Pending CN108841892A (en) | 2018-08-10 | 2018-08-10 | The method of Production by Enzymes gardenia red pigment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN108841892A (en) |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102304554A (en) * | 2011-06-01 | 2012-01-04 | 武汉绿孚生物工程有限责任公司 | Method for producing gardenia red pigment with high color value |
| WO2012043173A1 (en) * | 2010-09-27 | 2012-04-05 | 理研ビタミン株式会社 | Method for producing gardenia blue pigment |
| CN102732050A (en) * | 2012-06-06 | 2012-10-17 | 浙江科技学院 | Method for preparing gardenia pigments from Gardenia jasminoides Ellis |
-
2018
- 2018-08-10 CN CN201810909459.1A patent/CN108841892A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012043173A1 (en) * | 2010-09-27 | 2012-04-05 | 理研ビタミン株式会社 | Method for producing gardenia blue pigment |
| CN102304554A (en) * | 2011-06-01 | 2012-01-04 | 武汉绿孚生物工程有限责任公司 | Method for producing gardenia red pigment with high color value |
| CN102732050A (en) * | 2012-06-06 | 2012-10-17 | 浙江科技学院 | Method for preparing gardenia pigments from Gardenia jasminoides Ellis |
Non-Patent Citations (2)
| Title |
|---|
| 顾觉奋等: "《离子交换与吸附树脂在制药工业上的应用》", 30 April 2008, 中国医药科技出版社 * |
| 马伟光等: "《天然植物药的生物转化研究》", 31 May 2014, 云南科技出版社 * |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102732050B (en) | Method for preparing gardenia pigments from Gardenia jasminoides Ellis | |
| CN105949163B (en) | The method for extraction and purification of anthocyanidin in a kind of Black Box Tracing pomace | |
| CN101423538B (en) | Production process for extracting high-purity birutan from flos sophora | |
| CN103951718B (en) | A kind of method preparing high-purity gardenoside and crocin with cape jasmine | |
| CN101108842A (en) | Processing Technology of Extracting Tea Polyphenols from Tea Tree Flowers | |
| CN105061525A (en) | Preparation method of mono-ammonium glycyrrhizinate | |
| CN114014830A (en) | A kind of method for producing blueberry anthocyanins | |
| CN104630302A (en) | Enzyme process acylation method of strawberry anthocyanin | |
| CN102532334B (en) | Method for producing flaxseed mucilage | |
| CN106832045B (en) | A kind of method that gingko episperm extracts pectin and phenolic acid compound simultaneously | |
| CN108841892A (en) | The method of Production by Enzymes gardenia red pigment | |
| CN106543129A (en) | A kind of method of anthocyanidin in purifying black rice husk | |
| CN101475620A (en) | Efficient energy-saving extraction and production method for high-purity cordycepin | |
| CN101161111B (en) | Method for extracting sweet potato natural purple pigment | |
| CN103833805A (en) | Process for refining glycyrrhizinic acid in liquorice | |
| CN1927946A (en) | Extraction method of natural plant water-soluble red colouring matter | |
| CN109134178B (en) | A method for synchronously extracting lycopene and citrulline from watermelon | |
| CN104098636B (en) | A kind of method extracting rutin in the Flos Sophorae Immaturus | |
| CN102731463B (en) | A method of purifying anthocyanins in black currant | |
| CN114573725B (en) | Extraction method of spine date seed polysaccharide extract | |
| CN102492051A (en) | Polygonatum odoratum deep processing and comprehensive utilization process | |
| CN100389675C (en) | Extraction method of effective components of Pyracantha series | |
| CN110013508A (en) | A kind of Traditional Chinese medicinal liquor improving antitumor immunity | |
| CN104530170B (en) | A kind of method extracting astragaloside and Radix Astragali saponin V from the Radix Astragali | |
| CN107235951A (en) | A kind of new method of the high efficiency extraction anthocyanidin from black rice |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20181120 |