CN104542896A - Film-based composite mangosteen polyphenol chilled meat preservative and preparation method thereof - Google Patents
Film-based composite mangosteen polyphenol chilled meat preservative and preparation method thereof Download PDFInfo
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- CN104542896A CN104542896A CN201410798215.2A CN201410798215A CN104542896A CN 104542896 A CN104542896 A CN 104542896A CN 201410798215 A CN201410798215 A CN 201410798215A CN 104542896 A CN104542896 A CN 104542896A
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- ethyl acetate
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- 240000006053 Garcinia mangostana Species 0.000 title claims abstract description 196
- 235000017048 Garcinia mangostana Nutrition 0.000 title claims abstract description 196
- 235000013372 meat Nutrition 0.000 title claims abstract description 78
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 74
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 74
- 239000002131 composite material Substances 0.000 title claims abstract description 32
- 238000002360 preparation method Methods 0.000 title abstract description 33
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- 238000000034 method Methods 0.000 claims abstract description 37
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- 108010053775 Nisin Proteins 0.000 claims abstract description 28
- 239000004309 nisin Substances 0.000 claims abstract description 28
- 235000010297 nisin Nutrition 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- XEKOWRVHYACXOJ-UHFFFAOYSA-N Ethyl acetate Chemical compound CCOC(C)=O XEKOWRVHYACXOJ-UHFFFAOYSA-N 0.000 claims description 216
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 144
- 229920001282 polysaccharide Polymers 0.000 claims description 62
- 239000005017 polysaccharide Substances 0.000 claims description 62
- 150000004676 glycans Chemical class 0.000 claims description 58
- 239000000706 filtrate Substances 0.000 claims description 57
- 244000276331 Citrus maxima Species 0.000 claims description 53
- 235000001759 Citrus maxima Nutrition 0.000 claims description 53
- 239000003795 chemical substances by application Substances 0.000 claims description 44
- 230000032050 esterification Effects 0.000 claims description 44
- 238000005886 esterification reaction Methods 0.000 claims description 44
- 239000007788 liquid Substances 0.000 claims description 44
- 150000001875 compounds Chemical class 0.000 claims description 42
- 239000006228 supernatant Substances 0.000 claims description 41
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 36
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 36
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 36
- 239000012071 phase Substances 0.000 claims description 33
- 239000012528 membrane Substances 0.000 claims description 27
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 27
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 27
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 27
- 239000008346 aqueous phase Substances 0.000 claims description 26
- 238000000605 extraction Methods 0.000 claims description 26
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 24
- 230000018044 dehydration Effects 0.000 claims description 21
- 238000006297 dehydration reaction Methods 0.000 claims description 21
- 239000000284 extract Substances 0.000 claims description 18
- 239000013049 sediment Substances 0.000 claims description 18
- 239000003960 organic solvent Substances 0.000 claims description 16
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 15
- 230000001105 regulatory effect Effects 0.000 claims description 13
- 238000006243 chemical reaction Methods 0.000 claims description 12
- 239000000376 reactant Substances 0.000 claims description 12
- 238000007789 sealing Methods 0.000 claims description 12
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- 239000006286 aqueous extract Substances 0.000 claims description 9
- 238000002386 leaching Methods 0.000 claims description 8
- 238000010298 pulverizing process Methods 0.000 claims description 7
- 239000012074 organic phase Substances 0.000 claims description 6
- 108010059892 Cellulase Proteins 0.000 claims description 4
- 229940106157 cellulase Drugs 0.000 claims description 4
- AZHSSKPUVBVXLK-UHFFFAOYSA-N ethane-1,1-diol Chemical compound CC(O)O AZHSSKPUVBVXLK-UHFFFAOYSA-N 0.000 claims description 4
- 239000000835 fiber Substances 0.000 claims description 4
- 239000012466 permeate Substances 0.000 claims description 4
- -1 polysaccharide compound Chemical class 0.000 claims description 4
- 238000001556 precipitation Methods 0.000 claims description 4
- 238000003815 supercritical carbon dioxide extraction Methods 0.000 claims description 4
- 241000196324 Embryophyta Species 0.000 claims description 2
- 108010059820 Polygalacturonase Proteins 0.000 claims description 2
- 230000007071 enzymatic hydrolysis Effects 0.000 claims description 2
- 238000006047 enzymatic hydrolysis reaction Methods 0.000 claims description 2
- 108010093305 exopolygalacturonase Proteins 0.000 claims description 2
- 238000009472 formulation Methods 0.000 claims description 2
- 239000000758 substrate Substances 0.000 abstract description 8
- 235000016709 nutrition Nutrition 0.000 abstract description 3
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- 239000000796 flavoring agent Substances 0.000 abstract description 2
- 235000019634 flavors Nutrition 0.000 abstract description 2
- 235000019249 food preservative Nutrition 0.000 abstract description 2
- 239000005452 food preservative Substances 0.000 abstract description 2
- 244000005700 microbiome Species 0.000 abstract description 2
- 230000003064 anti-oxidating effect Effects 0.000 abstract 1
- LTUGGBOPBQPPGK-UHFFFAOYSA-A octadecasodium;hexaphosphate Chemical compound [Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[Na+].[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O.[O-]P([O-])([O-])=O LTUGGBOPBQPPGK-UHFFFAOYSA-A 0.000 abstract 1
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- Meat, Egg Or Seafood Products (AREA)
Abstract
The invention relates to the technical field of food preservatives, and particularly discloses a film-based composite mangosteen polyphenol chilled meat preservative and a preparation method thereof. The concentration of each component after being prepared into the water aqua is as follows: 0.5-1.5 g/L of mangosteen shell free phenol, 1.0-2.0 g/L of mangosteen shell esterified phenol, 0.5-1.0 g/L of mangosteen shell bound phenol, 0.02-0.07 g/L of nisin, 3-6 g/L of sodium hexaphosphate and 5-15 g/L of water-soluble film substrate. The film-based composite mangosteen polyphenol chilled fresh meat preservative can reduce the number of microorganisms on the surface of meat, prevent water from seeping out in the sale process of products, endow the products with a new anti-oxidation function, effectively prolong the shelf life of the chilled fresh meat and well ensure the nutrition and the flavor of the chilled fresh meat.
Description
Technical field
The present invention relates to food preservative technical field, be specifically related to cold fresh-keeping agent for meat of a kind of film base compound mangosteen polyphenol and preparation method thereof.
Background technology
In recent years, China Meat consumption there occurs the change of obvious structure, presents from chilled meat to Fresh meat, then from Fresh meat to the development trend of cold fresh meat, defines the general layout in " the wide world of Fresh meat, chilled meat is striven all over the world, and cold fresh meat is unsurpassed ".Cold fresh meat, is again Chilled Meats, acid discharge meat, chilled meat, and modal have cold fresh pork, cold fresh beef, cold fresh mutton, chilled fresh chicken etc.Developed country just started to promote cold fresh meat as far back as the eighties of last century twenty or thirty age, and in the fresh meat of developed country's consumption, cold fresh meat accounts for about 90%.But cold fresh meat exist shelf life short, sell the defects such as radius is little, extending its shelf life is expand the key of selling radius, is also the important channel that meat products that some have a region feature realizes being converted into from raw material advantage product advantage.The method of the fresh-keeping normal employing of meat controls holding conditions and chemical treatment.The method that the holding conditions of control meat is the most frequently used is low-temperature preservation, although meat can suppress most growth of microorganism under cryogenic, some psychrophiles still can grow under cryogenic, and it is corrupt to cause chilled meat to occur.And chemical method normally adds anticorrisive agent in meat products, but the side effect of chemical preservative more and more draws attention, and its range of application is also more restricted.The use of plant polyose composite antistaling agent will reduce the potential safety hazard that chemical preservative and other anti-corrosion mode bring largely.
Meat Middle nutrition enriches, and has higher water activity, for microbial growth provides good condition.From hurdle technology, usually all there is certain defect in single anticorrisive agent or preservation method, must adopt synthetical preservation technology, competence exertion complementation and the effect that is multiplied, the growth of retard microbial and other unfavorable factor effectively, the object reach mutual supplement with each other's advantages, bringing out the best in each other.Therefore a kind of complex biological preservative is developed necessary.
Summary of the invention
technical problem to be solved by this invention is, in order to overcome the guarantor of single component antistaling agent in prior art
The deficiency of fresh effect, provides cold fresh-keeping agent for meat of a kind of film base compound mangosteen polyphenol and preparation method thereof.
Above-mentioned technical problem to be solved by this invention is achieved by the following technical programs:
The cold fresh-keeping agent for meat of a kind of film base compound mangosteen polyphenol, comprises following component: mangosteen polyphenol, nisin, sodium hexametaphosphate, water-solubility membrane base.
As a kind of preferred version, the described cold fresh-keeping agent for meat of film base compound mangosteen polyphenol, comprises the component of following weight portion: mangosteen polyphenol 20 ~ 50 parts, nisin 0.2 ~ 0.7 part, sodium hexametaphosphate 30 ~ 60 parts, 50 ~ 150 parts, water-solubility membrane base.
As a kind of preferred version, described mangosteen polyphenol comprises described mangosteen polyphenol mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell in conjunction with state phenol.
As a kind of preferred version, the described cold fresh-keeping agent for meat of film base compound mangosteen polyphenol, comprises the component of following weight portion: 5 ~ 15 parts, mangosteen shell free state phenol, 10 ~ 20 parts, mangosteen shell esterification state phenol, mangosteen shell are in conjunction with 5 ~ 10 parts, state phenol, nisin 0.2 ~ 0.7 part, sodium hexametaphosphate 30 ~ 60 parts, 50 ~ 150 parts, water-solubility membrane base.
As the further preferred version of one, the described cold fresh-keeping agent for meat of film base compound mangosteen polyphenol, comprises the component of following weight portion: 8 ~ 12 parts, mangosteen shell free state phenol, 12 ~ 18 parts, mangosteen shell esterification state phenol, mangosteen shell are in conjunction with 6 ~ 10 parts, state phenol, nisin 0.4 ~ 0.6 part, sodium hexametaphosphate 40 ~ 60 parts, 80 ~ 120 parts, water-solubility membrane base.
As one most preferably scheme, the described cold fresh-keeping agent for meat of film base compound mangosteen polyphenol, comprises the component of following weight portion: 10 parts, mangosteen shell free state phenol, 15 parts, mangosteen shell esterification state phenol, mangosteen shell are in conjunction with 8 parts, state phenol, nisin 0.5 part, sodium hexametaphosphate 50 parts, 100 parts, water-solubility membrane base.
As a kind of preferred version, described mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell prepare by the following method in conjunction with state phenol:
(1) get dry mangosteen shell, after pulverizing, add methanol/acetone/aqueous extract by solid-liquid ratio 1g:10 ~ 30L, at room temperature lucifuge jolting is extracted, is filtered to get filtrate and filter residue, filtrate is concentrated into 1/4 ~ 1/6 of original volume, obtains concentrate; The pH value regulating concentrate is 2 ~ 3, centrifugal, obtains the supernatant of concentrated filtrate and the centrifugal sediment of concentrated filtrate; By concentrated filtrate supernatant n-hexane extraction degrease, then extract to obtain ethyl acetate/absolute ether phase and aqueous phase two parts with ethyl acetate/absolute ether; Finally by ethyl acetate/absolute ether phase dehydration, concentrated, obtain mangosteen shell free state phenol;
(2) aqueous phase after being extracted with concentrated filtrate supernatant ethyl acetate/absolute ether by the centrifugal sediment of the concentrated filtrate of step (1) mixes, and obtains the mixed liquor containing esterification state phenol; Add 3 ~ 5mol/L NaOH according to liquid liquor ratio 1:3 ~ 8, after sealing, lucifuge jolting reaction 3 ~ 4h, regulates reacting liquid pH value to be 2 ~ 3, centrifugal the supernatant of mixed liquor and the centrifugal sediment of mixed liquor; The supernatant n-hexane extraction degrease of mixed liquor, then with ethyl acetate/absolute ether extraction, obtain ethyl acetate/absolute ether phase and aqueous phase two parts; Finally by ethyl acetate/absolute ether phase dehydration, concentrated removing organic solvent, obtain mangosteen shell esterification state phenol;
(3) step (1) is pumped through the filter residue after filter and adds 3 ~ 5mol/L NaOH according to solid-liquid ratio 1g:3 ~ 8L, lucifuge jolting reaction 3 ~ 4h after sealing, reacting liquid pH value is regulated to be 2 ~ 3, the centrifugal supernatant obtaining filter residue reactant liquor, the supernatant n-hexane extraction degrease of filter residue reactant liquor, again with isopyknic ethyl acetate/absolute ether extraction, obtain ethyl acetate/absolute ether phase; Finally by ethyl acetate/absolute ether phase dehydration, concentrated removing organic solvent, obtain mangosteen shell in conjunction with state phenol.
As the further preferred version of one, mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell prepare by the following method in conjunction with state phenol:
(1) get dry mangosteen shell, after pulverizing, add methanol/acetone/aqueous extract by solid-liquid ratio 1g:20 ~ 30L, at room temperature lucifuge jolting is extracted 10 ~ 30min, is filtered to get filtrate and filter residue, filtrate is concentrated into 1/5 ~ 1/6 of original volume, obtains concentrate; The pH value regulating concentrate with 6mol/L HCl is 2 ~ 3, centrifugal, obtains the supernatant of concentrated filtrate and the centrifugal sediment of concentrated filtrate; By concentrated filtrate supernatant isopyknic n-hexane extraction 1 ~ 3 degrease, then with ethyl acetate/absolute ether extraction 1 ~ 3 time, merge organic phase and aqueous phase respectively, obtain ethyl acetate/absolute ether phase and aqueous phase two parts; Finally ethyl acetate/absolute ether is used anhydrous sodium sulfate dehydration mutually, more concentrated remove organic solvent, obtain mangosteen shell free state phenol;
(2) aqueous phase after being extracted with concentrated filtrate supernatant ethyl acetate/absolute ether by the centrifugal sediment of the concentrated filtrate of step (1) mixes, and obtains the mixed liquor containing esterification state phenol; Add 4 ~ 5mol/L NaOH according to liquid liquor ratio 1:5 ~ 8, after sealing, lucifuge jolting reaction 3 ~ 4h, regulates reacting liquid pH value to be 2 with HCl, centrifugal the supernatant of mixed liquor and the centrifugal sediment of mixed liquor; Supernatant equal-volume n-hexane extraction 1 ~ 3 degrease of mixed liquor, then with isopyknic ethyl acetate/absolute ether extraction 1 ~ 3 time, merge organic phase and aqueous phase respectively, obtain ethyl acetate/absolute ether phase and aqueous phase two parts; Finally ethyl acetate/absolute ether is used anhydrous sodium sulfate dehydration mutually, more concentrated removing organic solvent, obtain mangosteen shell esterification state phenol;
(3) step (1) is pumped through the filter residue after filter and adds 4mol/L NaOH according to solid-liquid ratio 1g:5 ~ 8L, lucifuge jolting reaction 3 ~ 4h after sealing, reacting liquid pH value is regulated to be 2 with 6mol/L HCl, the centrifugal supernatant obtaining filter residue reactant liquor, supernatant n-hexane extraction 1 ~ 3 degrease of filter residue reactant liquor, again with ethyl acetate/absolute ether extraction 1 ~ 3 time, obtain ethyl acetate/absolute ether phase; Finally ethyl acetate/absolute ether is used mutually anhydrous sodium sulfate dehydration, concentrated removing organic solvent, obtain mangosteen shell in conjunction with state phenol.
As one most preferably scheme, mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell prepare by the following method in conjunction with state phenol:
(1) get dry mangosteen shell, after pulverizing, add methanol/acetone/aqueous extract by solid-liquid ratio 1g:20L, at room temperature lucifuge jolting is extracted 10 ~ 30min, is filtered to get filtrate and filter residue, filtrate is concentrated into 1/5 of original volume, obtains concentrate; The pH value regulating concentrate with 6mol/L HCl is 2, centrifugal, obtains the supernatant of concentrated filtrate and the centrifugal sediment of concentrated filtrate; By concentrated filtrate supernatant isopyknic n-hexane extraction 3 degreases, then extract 3 times with ethyl acetate/absolute ether, merge organic phase and aqueous phase respectively, obtain ethyl acetate/absolute ether phase and aqueous phase two parts; Finally ethyl acetate/absolute ether is used anhydrous sodium sulfate dehydration mutually, more concentrated remove organic solvent, obtain mangosteen shell free state phenol;
(2) aqueous phase after being extracted with concentrated filtrate supernatant ethyl acetate/absolute ether by the centrifugal sediment of the concentrated filtrate of step (1) mixes, and obtains the mixed liquor containing esterification state phenol; Add 4mol/L NaOH according to liquid liquor ratio 1:5, after sealing, lucifuge jolting reaction 4h, regulates reacting liquid pH value to be 2 with 6mol/LHCl, centrifugal the supernatant of mixed liquor and the centrifugal sediment of mixed liquor; Supernatant equal-volume n-hexane extraction 3 degreases of mixed liquor, then extract 3 times with isopyknic ethyl acetate/absolute ether, merge organic phase and aqueous phase respectively, obtain ethyl acetate/absolute ether phase and aqueous phase two parts; Finally ethyl acetate/absolute ether is used anhydrous sodium sulfate dehydration mutually, more concentrated removing organic solvent, obtain mangosteen shell esterification state phenol;
(3) step (1) is pumped through the filter residue after filter and adds 4mol/L NaOH according to solid-liquid ratio 1g:5 L, lucifuge jolting reaction 4h after sealing, reacting liquid pH value is regulated to be 2 with 6mol/L HCl, the centrifugal supernatant obtaining filter residue reactant liquor, supernatant n-hexane extraction 3 degreases of filter residue reactant liquor, extract 3 times with ethyl acetate/absolute ether again, obtain ethyl acetate/absolute ether phase; Finally ethyl acetate/absolute ether is used mutually anhydrous sodium sulfate dehydration, concentrated removing organic solvent, obtain mangosteen shell in conjunction with state phenol;
As a kind of preferred version, the methanol/acetone/aqueous extract described in step (1), the volume ratio of methyl alcohol wherein, acetone and water is 5 ~ 7:5 ~ 7:5 ~ 6; Ethyl acetate/absolute ether used in extraction process in step (1), (2) and (3), wherein, wherein the volume ratio of ethyl acetate and absolute ether is 1 ~ 2:1 ~ 2.
As one most preferably scheme, the methanol/acetone/aqueous extract described in step (1), the volume ratio of methyl alcohol wherein, acetone and water is 7:7:6; Ethyl acetate/absolute ether used in extraction process in step (1), (2) and (3), wherein, wherein the volume ratio of ethyl acetate and absolute ether is 1:1.
The polyphenol obtained by additive method also can realize the present invention.But the mangosteen shell free state phenol prepared through the inventive method, mangosteen shell esterification state phenol, mangosteen shell are applied in antistaling agent of the present invention in conjunction with state phenol has better anticorrosion and fresh-keeping effect.
As a kind of preferred version, described water-solubility membrane base comprises Pul and shaddock ped polysaccharide, and wherein Pul and shaddock ped polysaccharide compound proportion are 1:3 ~ 3:1.
As one most preferably scheme, Pul and shaddock ped polysaccharide compound proportion are 1:3.
As the further preferred version of one, described shaddock ped polysaccharide prepares by the following method: shaddock ped is extracted ungrease treatment through supercritical carbon dioxide extraction equipment, then soak first time shaddock ped leaching liquor; Will first time shaddock ped leaching liquor cellulase and pectinase enzymatic hydrolysis, centrifugal, filter; Filtrate is crossed the hollow-fibre membrane that molecular cut off is 100,000 again, collect permeate, obtain shaddock ped extract; Be 40 ~ 80% ethanol alcohol precipitations respectively by shaddock ped extract volume fraction, obtain 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c; 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c are obtained shaddock ped polysaccharide so that the ratio of weight ratio 1:3:2 ~ 3:1:2 is composite; Preferably, 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c obtain shaddock ped polysaccharide so that the ratio of weight ratio 1:2:1 is composite.Extract by additive method the shaddock ped polysaccharide obtained and also can realize the present invention, but the shaddock ped polysaccharide obtained by preparation method of the present invention is applied in antistaling agent of the present invention has better anticorrisive agent fresh-keeping effect.
As one most preferably scheme, described shaddock ped polysaccharide prepares by the following method: choose the shaddock of harvesting in fresh autumn, peeling, drying, pulverizing, with supercritical carbon dioxide extraction equipment ungrease treatment 60 minutes, and pressure 45MPa, temperature 45 C, CO
2flow 30L/h; In kg/L after ungrease treatment, add the distilled water that mass volume ratio is 1:10 ~ 20, soak 30min, obtain first time shaddock ped leaching liquor; In shaddock ped first leaching liquor, add acid for adjusting pH value is 3.0 ~ 4.0, by heating temperatures to 45 ~ 55 DEG C, adds 4 ~ 6g cellulase and pectase (1:2) in every kg shaddock ped respectively, and after ultrasound-assisted enzymolysis 2 ~ 3h, enzyme-deactivating is carried out in heating.Then extract Horizontal helical type centrifuge carries out Separation of Solid and Liquid with the speed of 1800 ~ 2000r/min, collects filtrate and residue, obtains the first filtrate; Residue is added the distilled water that mass volume ratio is 1:5 ~ 10 again, soak 30min, after ultrasonic wave process 2-3h, centrifugal, collect filtrate, obtain the second filtrate, mix described first filtrate and the second filtrate, this mixing filtrate is crossed the hollow-fibre membrane that molecular cut off is 100,000, collects permeate through reduced pressure concentration, obtain shaddock ped extract; Be 40 ~ 80% ethanol alcohol precipitations respectively by shaddock ped extract volume fraction, after vacuum freeze-drying, be ground into 60 order pressed powders, obtain 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c; 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c are obtained shaddock ped polysaccharide so that the ratio of weight ratio 1:2:1 is composite;
As a kind of preferred version, the formulation of the described cold fresh-keeping agent for meat of film base compound mangosteen polyphenol is aqua form, and wherein the concentration of each component is: mangosteen shell free state phenol 0.5 ~ 1.5g/L, mangosteen shell esterification state phenol 1.0 ~ 2.0g/L, mangosteen shell are in conjunction with state phenol 0.5 ~ 1.0 g/L, nisin 0.02 ~ 0.07 g/L, sodium hexametaphosphate 3 ~ 6 g/L, water-solubility membrane base 5 ~ 15 g/L.
As the further preferred version of one, described cold fresh-keeping agent for meat of film base compound mangosteen polyphenol and preparation method thereof, comprises the component of following weight portion: mangosteen shell free state phenol 0.8 ~ 1.2g/L, mangosteen shell esterification state phenol 1.2 ~ 1.8 g/L, mangosteen shell are in conjunction with 0.6 ~ 1.0 part, state phenol, nisin 0.04 ~ 0.06 g/L, sodium hexametaphosphate 4 ~ 6 g/L, water-solubility membrane base 8 ~ 12 g/L.
As one most preferably scheme, described cold fresh-keeping agent for meat of film base compound mangosteen polyphenol and preparation method thereof, comprises the component of following weight portion: mangosteen shell free state phenol 1.0g/L, mangosteen shell esterification state phenol 1.5g/L, mangosteen shell are in conjunction with state phenol 0.8 g/L, nisin 0.05 g/L, sodium hexametaphosphate 5g/L, water-solubility membrane base 10g/L.
As a kind of preferred version, described mangosteen polyphenol comprises mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell in conjunction with state phenol one-component or blending ingredients.
The preparation method of the cold fresh-keeping agent for meat aqua of described film base compound mangosteen polyphenol is:
(1) get mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell be dissolved in distilled water in conjunction with state phenol and be mixed with mangosteen polyphenol composite solution.Get mass fraction 65 ~ 75% above-mentioned mangosteen polyphenol composite solution, add film base material material (Pul and shaddock ped polysaccharide ratio are 1:3 ~ 3:1) while stirring, be stirred to film substrate matter and all dissolve, obtained film based sols;
(2) shaddock ped polysaccharide, sodium hexametaphosphate are mixed with nisin, then mix with remaining mangosteen polyphenol composite solution, be stirred well to dissolving, obtained streptococcus lactis cellulose solution;
(3) film based sols is mixed with streptococcus lactis cellulose solution be the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol and preparation method thereof aqua.
Beneficial effect: water-solubility membrane base, natural antiseptic agent, natural are carried out science combination and obtain a kind of brand-new natural refrigerated fresh meat composite preservative by the present invention, advantage is simple to operate, not only improve antistaling agent anti-microbial property, and give its oxidation resistant New function, effectively can extend the shelf life of cold fresh meat, ensure nutrition and the local flavor of cold fresh meat well.
Detailed description of the invention
Explain the present invention further below in conjunction with specific embodiment, but embodiment does not limit in any form to invention.
Embodiment 1
By mangosteen shell free state phenol 0.5g, mangosteen shell esterification state phenol 2.0g, mangosteen shell in conjunction with state phenol 0.5g, nisin 0.05 g, sodium hexametaphosphate 3 g, water-solubility membrane base 10 g, distilled water 1L, the aqua of cold fresh-keeping agent for meat of preparation film forming base compound mangosteen polyphenol and preparation method thereof.
Compound method:
(1) get mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell be dissolved in distilled water in conjunction with state phenol and be mixed with mangosteen polyphenol composite solution.Get mass fraction 65% above-mentioned mangosteen polyphenol composite solution, add film base material material (Pul and shaddock ped polysaccharide ratio are 1:3) while stirring, be stirred to film substrate matter and all dissolve, obtained film based sols;
(2) sodium hexametaphosphate is mixed with nisin, then mix with remaining mangosteen polyphenol composite solution, be stirred well to dissolving, obtained streptococcus lactis cellulose solution;
(3) film based sols is mixed with streptococcus lactis cellulose solution be the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol and preparation method thereof aqua.
In the present embodiment, mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell prepare by the following method in conjunction with state phenol: (1) learns from else's experience the mangosteen shell of natural drying, to pulverize with mechanical crushing equipment and after crossing 20 mesh sieves, methanol/acetone/aqueous extract (7:7:6 is added by solid-liquid ratio 1:20 (g/L), v/v/v), 10-30min is extracted at room temperature lucifuge jolting, suction filtration, and filter residue as above repeats extraction 3 times, merging filtrate, filter residue is for subsequent use.Adopt Rotary Evaporators by filter vacuum concentrated (45 DEG C) to certain volume (cycles of concentration is 5), concentrated filtrate pH value is regulated to be 2 with 6mol/L HCl, centrifugal (6000r/min, 15min, 4 DEG C), obtain the supernatant of concentrated filtrate and the centrifugal sediment of concentrated filtrate.Isopyknic n-hexane (the 1:1 of concentrated filtrate supernatant, v/v) after degrease 3 times, then equal-volume ethyl acetate/absolute ether (1/1, v/v) is used to extract 3 times, combined ethyl acetate/absolute ether phase and aqueous phase, obtain ethyl acetate/absolute ether phase and aqueous phase two parts respectively.Adopt anhydrous sodium sulfate to above-mentioned ethyl acetate/absolute ether phase dehydration, finally the ethyl acetate after anhydrous sodium sulfate dehydration/absolute ether phase Vacuum Concentration (30 DEG C) is removed organic solvent, obtain mangosteen shell free state phenol.
(2) aqueous phase after being extracted with ethyl acetate/absolute ether by the centrifugal sediment of the concentrated filtrate of step (1) mixes, obtain the mixed liquor containing esterification state phenol, 4mol/L NaOH is added according to liquid liquor ratio (1:5), lucifuge jolting reaction 4h after sealing, reacting liquid pH value is regulated to be 2 with 6mol/LHCl, centrifugal (6000r/min, 15min, 4 DEG C), obtain the supernatant of mixed liquor and the centrifugal sediment of mixed liquor.Isopyknic n-hexane (the 1:1 of supernatant of mixed liquor, v/v) after degrease 3 times, then equal-volume ethyl acetate/absolute ether (1/1, v/v) is used to extract 3 times, combined ethyl acetate/absolute ether phase and aqueous phase, obtain ethyl acetate/absolute ether phase and aqueous phase two parts respectively.Adopt anhydrous sodium sulfate to above-mentioned ethyl acetate/absolute ether phase dehydration, finally the ethyl acetate after anhydrous sodium sulfate dehydration/absolute ether phase Vacuum Concentration (30 DEG C) is removed organic solvent, obtain mangosteen shell esterification state phenol.
(3) filter residue after step (1) suction filtration is added 4mol/L NaOH according to solid-liquid ratio (1:5), lucifuge jolting reaction 4h after sealing, reacting liquid pH value is regulated to be 2 with 6mol/L HCl, centrifugal (6000r/min, 15min, 4 DEG C), obtain the supernatant of filter residue reactant liquor, isopyknic n-hexane (the 1:1 of supernatant of filter residue reactant liquor, v/v) after degrease 3 times, then equal-volume ethyl acetate/absolute ether (1:1, v/v) is used to extract 3 times, combined ethyl acetate/absolute ether phase, obtains ethyl acetate/absolute ether phase.Adopt anhydrous sodium sulfate to above-mentioned ethyl acetate/absolute ether phase dehydration, finally the ethyl acetate after anhydrous sodium sulfate dehydration/absolute ether phase Vacuum Concentration (30 DEG C) is removed organic solvent, namely obtain mangosteen shell in conjunction with state phenol.
Shaddock ped polysaccharide of the present invention prepares by the following method: choose the shaddock of harvesting in fresh autumn, peeling, drying, pulverizing, with supercritical carbon dioxide extraction equipment ungrease treatment 60 minutes, and pressure 45MPa, temperature 45 C, CO
2flow 30L/h; In kg/L after ungrease treatment, add the distilled water that mass volume ratio is 1:20, soak 30min, obtain first time shaddock ped leaching liquor; In shaddock ped first leaching liquor, add acid for adjusting pH value is 3.0 ~ 4.0, by heating temperatures to 45 ~ 55 DEG C, adds 4 ~ 6g cellulase and pectase (1:2) in every kg shaddock ped respectively, and after ultrasound-assisted enzymolysis 3h, enzyme-deactivating is carried out in heating.Then extract Horizontal helical type centrifuge carries out Separation of Solid and Liquid with the speed of 1800 ~ 2000r/min, collects filtrate and residue, obtains the first filtrate; Residue is added the distilled water that mass volume ratio is 1:10 again, soak 30min, after ultrasonic wave process 2-3h, centrifugal, collect filtrate, obtain the second filtrate, mix described first filtrate and the second filtrate, this mixing filtrate is crossed the hollow-fibre membrane that molecular cut off is 100,000, collect permeate through reduced pressure concentration, obtaining shaddock ped extract volume fraction is 40 ~ 80% ethanol alcohol precipitations respectively, is ground into 60 order pressed powders, obtains 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c after vacuum freeze-drying; 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c are obtained shaddock ped polysaccharide so that the ratio of weight ratio 1:2:1 is composite;
embody rule is tested:by the pork of newly butchering at-18 DEG C freezing 1 hour, then 2 DEG C of refrigerations 8 hours, make the near 0-4 DEG C of its central temperature.In advance by cutter used and chopping board through 75% alcohol disinfecting sterilization and ultraviolet irradiation 15min, under sterile working, shave off the manadesma of pork and unnecessary fat, be cut into 25g(to test for total number of bacteria) and 50g (for other index Tests) left and right cube meat, divide into groups immediately, use fresh-keeping liquid process respectively, namely in fresh-keeping liquid, soak 2min, taking-up drains in rear loading PE freshness protection package, preserves and measure total number of bacteria, TVB-N value in 7 days in 0-4 DEG C of refrigerator.Bacterium sum measures: measure according to 4789.2-2010 food microbiological examination-total plate count method for measuring.TVB-N pH-value determination pH: measure by the microdiffusion in the analytical method of GB/T5009-44-2003 meat quail sanitary standard.
testing result shows:within 7 days, the logarithm of the total number of bacteria of the present embodiment rises to 4.9, TVB-N value by 3.2 and rises to 10.1mg/100g by 6.6mg/100g; Blank total number of bacteria rises to 7.13, TVB-N value by 3.2 and is risen by 6.6mg/100g, 21.8mg/100g.
Embodiment 2
By mangosteen shell free state phenol 1.0g, mangosteen shell esterification state phenol 1.5 g, mangosteen shell in conjunction with state phenol 0.5 g, nisin 0.02g, sodium hexametaphosphate 4g, water-solubility membrane base 15 g, distilled water 1L, the aqua of cold fresh-keeping agent for meat of preparation film forming base compound mangosteen polyphenol and preparation method thereof.Wherein the preparation method of mangosteen polyphenol and shaddock ped polysaccharide is with embodiment 1.
Compound method:
(1) get mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell be dissolved in distilled water in conjunction with state phenol and be mixed with mangosteen polyphenol composite solution.Get mass fraction 70% above-mentioned mangosteen polyphenol composite solution, add film base material material (Pul and shaddock ped polysaccharide ratio are 2:3) while stirring, be stirred to film substrate matter and all dissolve, obtained film based sols;
(2) sodium hexametaphosphate is mixed with nisin, then mix with remaining mangosteen polyphenol composite solution, be stirred well to dissolving, obtained streptococcus lactis cellulose solution;
(3) film based sols is mixed with streptococcus lactis cellulose solution be the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol and preparation method thereof aqua.
embody rule is tested:by the pork of newly butchering at-18 DEG C freezing 1 hour, then 2 DEG C of refrigerations 8 hours, make the near 0-4 DEG C of its central temperature.In advance by cutter used and chopping board through 75% alcohol disinfecting sterilization and ultraviolet irradiation 15min, under sterile working, shave off the manadesma of pork and unnecessary fat, be cut into 25g(to test for total number of bacteria) and 50g (for other index Tests) left and right cube meat, divide into groups immediately, use fresh-keeping liquid process respectively, namely in fresh-keeping liquid, soak 2min, taking-up drains in rear loading PE freshness protection package, preserves and measure total number of bacteria, TVB-N value in 7 days in 0-4 DEG C of refrigerator.Bacterium sum measures: measure according to 4789.2-2010 food microbiological examination-total plate count method for measuring.TVB-N pH-value determination pH: measure by the microdiffusion in the analytical method of GB/T5009-44-2003 meat quail sanitary standard.
testing result shows:within 7 days, the logarithm of the total number of bacteria of the present embodiment rises to 4.95, TVB-N value by 3.2 and rises to 9.35mg/100g by 6.7mg/100g; Blank total number of bacteria rises to 6.01, TVB-N value by 3.2 and rises to 20.1mg/100g by 6.7mg/100g.
Embodiment 3
By mangosteen shell free state phenol 0.8g, mangosteen shell esterification state phenol 1.5 g, mangosteen shell in conjunction with state phenol 0.5 g, nisin 0.06 g, sodium hexametaphosphate 3g, water-solubility membrane base 13 g, distilled water 1L, the aqua of cold fresh-keeping agent for meat of preparation film forming base compound mangosteen polyphenol and preparation method thereof.Wherein the preparation method of mangosteen polyphenol and shaddock ped polysaccharide is with embodiment 1.
Compound method:
(1) get mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell be dissolved in distilled water in conjunction with state phenol and be mixed with mangosteen polyphenol composite solution.Get mass fraction 75% above-mentioned mangosteen polyphenol composite solution, add film base material material (Pul and shaddock ped polysaccharide ratio are 3:1) while stirring, be stirred to film substrate matter and all dissolve, obtained film based sols;
(2) sodium hexametaphosphate is mixed with nisin, then mix with remaining mangosteen polyphenol composite solution, be stirred well to dissolving, obtained streptococcus lactis cellulose solution;
(3) film based sols is mixed with streptococcus lactis cellulose solution be the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol and preparation method thereof aqua.
embody rule is tested:by the pork of newly butchering at-18 DEG C freezing 1 hour, then 2 DEG C of refrigerations 8 hours, make the near 0-4 DEG C of its central temperature.In advance by cutter used and chopping board through 75% alcohol disinfecting sterilization and ultraviolet irradiation 15min, under sterile working, shave off the manadesma of pork and unnecessary fat, be cut into 25g(to test for total number of bacteria) and 50g (for other index Tests) left and right cube meat, divide into groups immediately, use fresh-keeping liquid process respectively, namely in fresh-keeping liquid, soak 2min, taking-up drains in rear loading PE freshness protection package, preserves and measure total number of bacteria, TVB-N value in 7 days in 0-4 DEG C of refrigerator.Bacterium sum measures: measure according to 4789.2-2010 food microbiological examination-total plate count method for measuring.TVB-N pH-value determination pH: measure by the microdiffusion in the analytical method of GB/T5009-44-2003 meat quail sanitary standard.
Testing result shows: within 7 days, the logarithm of the total number of bacteria of the present embodiment rises to 5.1, TVB-N value by 3.2 and rises to 10.3mg/100g by 6.7mg/100g; Blank total number of bacteria rises to 6.79, TVB-N value by 3.2 and rises to 20.9mg/100g by 6.7mg/100g.
Embodiment 4
By mangosteen shell free state phenol 0.75g, mangosteen shell esterification state phenol 1.5 g, mangosteen shell in conjunction with state phenol 0.8g, nisin 0.045 g, sodium hexametaphosphate 4.5g, water-solubility membrane base 10g, distilled water 1L, the aqua of cold fresh-keeping agent for meat of preparation film forming base compound mangosteen polyphenol and preparation method thereof.Wherein the preparation method of mangosteen polyphenol and shaddock ped polysaccharide is with embodiment 1.
Compound method:
(1) get mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell be dissolved in distilled water in conjunction with state phenol and be mixed with mangosteen polyphenol composite solution.Get mass fraction 75% above-mentioned mangosteen polyphenol composite solution, add film base material material (Pul and shaddock ped polysaccharide ratio are 3:2) while stirring, be stirred to film substrate matter and all dissolve, obtained film based sols;
(2) sodium hexametaphosphate is mixed with nisin, then mix with remaining mangosteen polyphenol composite solution, be stirred well to dissolving, obtained streptococcus lactis cellulose solution;
(3) film based sols is mixed with streptococcus lactis cellulose solution be the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol and preparation method thereof aqua.
embody rule is tested:by the pork of newly butchering at-18 DEG C freezing 1 hour, then 2 DEG C of refrigerations 8 hours, make the near 0-4 DEG C of its central temperature.In advance by cutter used and chopping board through 75% alcohol disinfecting sterilization and ultraviolet irradiation 15min, under sterile working, shave off the manadesma of pork and unnecessary fat, be cut into 25g(to test for total number of bacteria) and 50g (for other index Tests) left and right cube meat, divide into groups immediately, use fresh-keeping liquid process respectively, namely in fresh-keeping liquid, soak 2min, taking-up drains in rear loading PE freshness protection package, preserves and measure total number of bacteria, TVB-N value in 7 days in 0-4 DEG C of refrigerator.Bacterium sum measures: measure according to 4789.2-2010 food microbiological examination-total plate count method for measuring.TVB-N pH-value determination pH: measure by the microdiffusion in the analytical method of GB/T5009-44-2003 meat quail sanitary standard.
testing result shows:testing result shows: within 7 days, the logarithm of the total number of bacteria of the present embodiment rises to 4.98, TVB-N value by 3.2 and rises to 9.93mg/100g by 6.7mg/100g; Blank total number of bacteria rises to 6.82, TVB-N value by 3.2 and rises to 20.1mg/100g by 6.7mg/100g.
Embodiment 5
By mangosteen shell free state phenol 0.8g, mangosteen shell esterification state phenol 1.5 g, mangosteen shell in conjunction with state phenol 1.0g, nisin 0.07g, sodium hexametaphosphate 6g, water-solubility membrane base 15 g, distilled water 1L, the aqua of cold fresh-keeping agent for meat of preparation film forming base compound mangosteen polyphenol and preparation method thereof.Wherein the preparation method of mangosteen polyphenol and shaddock ped polysaccharide is with embodiment 1.
Compound method:
(1) get mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell be dissolved in distilled water in conjunction with state phenol and be mixed with mangosteen polyphenol composite solution.Get mass fraction 75% above-mentioned mangosteen polyphenol composite solution, add film base material material (Pul and shaddock ped polysaccharide ratio are 1:3) while stirring, be stirred to film substrate matter and all dissolve, obtained film based sols;
(2) sodium hexametaphosphate is mixed with nisin, then mix with remaining mangosteen polyphenol composite solution, be stirred well to dissolving, obtained streptococcus lactis cellulose solution;
(3) film based sols is mixed with streptococcus lactis cellulose solution be the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol and preparation method thereof aqua.
embody rule is tested:by the pork of newly butchering at-18 DEG C freezing 1 hour, then 2 DEG C of refrigerations 8 hours, make the near 0-4 DEG C of its central temperature.In advance by cutter used and chopping board through 75% alcohol disinfecting sterilization and ultraviolet irradiation 15min, under sterile working, shave off the manadesma of pork and unnecessary fat, be cut into 25g(to test for total number of bacteria) and 50g (for other index Tests) left and right cube meat, divide into groups immediately, use fresh-keeping liquid process respectively, namely in fresh-keeping liquid, soak 2min, taking-up drains in rear loading PE freshness protection package, preserves and measure total number of bacteria, TVB-N value in 7 days in 0-4 DEG C of refrigerator.Bacterium sum measures: measure according to 4789.2-2010 food microbiological examination-total plate count method for measuring.TVB-N pH-value determination pH: measure by the microdiffusion in the analytical method of GB/T5009-44-2003 meat quail sanitary standard.
testing result shows:testing result shows: within 7 days, the logarithm of the total number of bacteria of the present embodiment rises to 4.99, TVB-N value by 3.2 and rises to 9.93mg/100g by 6.7mg/100g; Blank total number of bacteria rises to 6.81, TVB-N value by 3.2 and rises to 19.9mg/100g by 6.7mg/100g.
Embodiment 6
By mangosteen shell free state phenol 1.0g, mangosteen shell esterification state phenol 1.5g, mangosteen shell in conjunction with state phenol 0.8g, nisin 0.05g, sodium hexametaphosphate 5.0g, water-solubility membrane base 10g, distilled water 1L, the aqua of cold fresh-keeping agent for meat of preparation film forming base compound mangosteen polyphenol and preparation method thereof.Wherein the preparation method of mangosteen polyphenol and shaddock ped polysaccharide is with embodiment 1.
Compound method:
(1) get mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell be dissolved in distilled water in conjunction with state phenol and be mixed with mangosteen polyphenol composite solution.Get mass fraction 70% above-mentioned mangosteen polyphenol composite solution, add film base material material (Pul and shaddock ped polysaccharide ratio are 1:2) while stirring, be stirred to film substrate matter and all dissolve, obtained film based sols;
(2) sodium hexametaphosphate is mixed with nisin, then mix with remaining mangosteen polyphenol composite solution, be stirred well to dissolving, obtained streptococcus lactis cellulose solution;
(3) film based sols is mixed with streptococcus lactis cellulose solution be the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol and preparation method thereof aqua.
embody rule is tested:by the pork of newly butchering at-18 DEG C freezing 1 hour, then 2 DEG C of refrigerations 8 hours, make the near 0-4 DEG C of its central temperature.In advance by cutter used and chopping board through 75% alcohol disinfecting sterilization and ultraviolet irradiation 15min, under sterile working, shave off the manadesma of pork and unnecessary fat, be cut into 25g(to test for total number of bacteria) and 50g (for other index Tests) left and right cube meat, divide into groups immediately, use fresh-keeping liquid process respectively, namely in fresh-keeping liquid, soak 2min, taking-up drains in rear loading PE freshness protection package, preserves and measure total number of bacteria, TVB-N value in 7 days in 0-4 DEG C of refrigerator.Bacterium sum measures: measure according to 4789.2-2010 food microbiological examination-total plate count method for measuring.TVB-N pH-value determination pH: measure by the microdiffusion in the analytical method of GB/T5009-44-2003 meat quail sanitary standard.
Testing result shows: testing result shows: within 7 days, the logarithm of the total number of bacteria of the present embodiment rises to 4.7, TVB-N value by 3.2 and rises to 9.3mg/100g by 6.7mg/100g; Blank total number of bacteria rises to 6.80, TVB-N value by 3.2 and rises to 19.8mg/100g by 6.7mg/100g.
Claims (10)
1. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol, is characterized in that, comprise following component: mangosteen polyphenol, nisin, sodium hexametaphosphate, water-solubility membrane base.
2. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol according to claim 1, it is characterized in that, comprise the component of following weight portion: mangosteen polyphenol 20 ~ 50 parts, nisin 0.2 ~ 0.7 part, sodium hexametaphosphate 30 ~ 60 parts, 50 ~ 150 parts, water-solubility membrane base; Preferably, described mangosteen polyphenol comprises mangosteen shell free state phenol, mangosteen shell esterification state phenol, mangosteen shell in conjunction with state phenol.
3. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol according to claim 2, it is characterized in that, comprise the component of following weight portion: 8 ~ 12 parts, mangosteen shell free state phenol, 12 ~ 18 parts, mangosteen shell esterification state phenol, mangosteen shell are in conjunction with 6 ~ 10 parts, state phenol, nisin 0.4 ~ 0.6 part, sodium hexametaphosphate 40 ~ 60 parts, 80 ~ 120 parts, water-solubility membrane base.
4. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol according to claim 2, it is characterized in that, comprise the component of following weight portion: 10 parts, mangosteen shell free state phenol, 15 parts, mangosteen shell esterification state phenol, mangosteen shell are in conjunction with 8 parts, state phenol, nisin 0.5 part, sodium hexametaphosphate 50 parts, 100 parts, water-solubility membrane base.
5. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol according to claim 1, is characterized in that, described mangosteen shell free state phenol, mangosteen shell esterification state phenol and mangosteen shell prepare by the following method in conjunction with state phenol:
(1) get dry mangosteen shell, after pulverizing, add methanol/acetone/aqueous extract by solid-liquid ratio 1g:10 ~ 30L, at room temperature lucifuge jolting is extracted, is filtered to get filtrate and filter residue, filtrate is concentrated into 1/4 ~ 1/6 of original volume, obtains concentrate; The pH value regulating concentrate is 2 ~ 3, centrifugal, obtains the supernatant of concentrated filtrate and the centrifugal sediment of concentrated filtrate; By concentrated filtrate supernatant n-hexane extraction degrease, then extract to obtain ethyl acetate/absolute ether phase and aqueous phase two parts with ethyl acetate/absolute ether; Finally by ethyl acetate/absolute ether phase dehydration, concentrated, obtain mangosteen shell free state phenol;
(2) aqueous phase after being extracted with concentrated filtrate supernatant ethyl acetate/absolute ether by the centrifugal sediment of the concentrated filtrate of step (1) mixes, and obtains the mixed liquor containing esterification state phenol; Add 3 ~ 5mol/L NaOH according to liquid liquor ratio 1:3 ~ 8, after sealing, lucifuge jolting reaction 3 ~ 4h, regulates reacting liquid pH value to be 2 ~ 3, centrifugal the supernatant of mixed liquor and the centrifugal sediment of mixed liquor; The supernatant n-hexane extraction degrease of mixed liquor, then with ethyl acetate/absolute ether extraction, obtain ethyl acetate/absolute ether phase and aqueous phase two parts; Finally by ethyl acetate/absolute ether phase dehydration, concentrated removing organic solvent, obtain mangosteen shell esterification state phenol;
(3) step (1) is pumped through the filter residue after filter and adds 3 ~ 5mol/L NaOH according to solid-liquid ratio 1g:3 ~ 8L, lucifuge jolting reaction 3 ~ 4h after sealing, reacting liquid pH value is regulated to be 2 ~ 3, the centrifugal supernatant obtaining filter residue reactant liquor, the supernatant n-hexane extraction degrease of filter residue reactant liquor, again with isopyknic ethyl acetate/absolute ether extraction, obtain ethyl acetate/absolute ether phase; Finally by ethyl acetate/absolute ether phase dehydration, concentrated removing organic solvent, obtain mangosteen shell in conjunction with state phenol.
6. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol according to claim 5, is characterized in that,
(1) get dry mangosteen shell, after pulverizing, add methanol/acetone/aqueous extract by solid-liquid ratio 1g:20L, at room temperature lucifuge jolting is extracted 10 ~ 30min, is filtered to get filtrate and filter residue, filtrate is concentrated into 1/5 of original volume, obtains concentrate; The pH value regulating concentrate with 6mol/L HCl is 2, centrifugal, obtains the supernatant of concentrated filtrate and the centrifugal sediment of concentrated filtrate; By concentrated filtrate supernatant isopyknic n-hexane extraction 3 degreases, then extract 3 times with ethyl acetate/absolute ether, merge organic phase and aqueous phase respectively, obtain ethyl acetate/absolute ether phase and aqueous phase two parts; Finally ethyl acetate/absolute ether is used anhydrous sodium sulfate dehydration mutually, more concentrated remove organic solvent, obtain mangosteen shell free state phenol;
(2) aqueous phase after being extracted with concentrated filtrate supernatant ethyl acetate/absolute ether by the centrifugal sediment of the concentrated filtrate of step (1) mixes, and obtains the mixed liquor containing esterification state phenol; Add 4mol/L NaOH according to liquid liquor ratio 1:5, after sealing, lucifuge jolting reaction 4h, regulates reacting liquid pH value to be 2 with 6mol/LHCl, centrifugal the supernatant of mixed liquor and the centrifugal sediment of mixed liquor; Supernatant equal-volume n-hexane extraction 3 degreases of mixed liquor, then extract 3 times with isopyknic ethyl acetate/absolute ether, merge organic phase and aqueous phase respectively, obtain ethyl acetate/absolute ether phase and aqueous phase two parts; Finally ethyl acetate/absolute ether is used anhydrous sodium sulfate dehydration mutually, more concentrated removing organic solvent, obtain mangosteen shell esterification state phenol;
(3) step (1) is pumped through the filter residue after filter and adds 4mol/L NaOH according to solid-liquid ratio 1g:5 L, lucifuge jolting reaction 4h after sealing, reacting liquid pH value is regulated to be 2 with 6mol/L HCl, the centrifugal supernatant obtaining filter residue reactant liquor, supernatant n-hexane extraction 3 degreases of filter residue reactant liquor, extract 3 times with ethyl acetate/absolute ether again, obtain ethyl acetate/absolute ether phase; Finally ethyl acetate/absolute ether is used mutually anhydrous sodium sulfate dehydration, concentrated removing organic solvent, obtain mangosteen shell in conjunction with state phenol;
Preferably, the methanol/acetone/aqueous extract described in step (1), the volume ratio of methyl alcohol wherein, acetone and water is 7:7:6; Ethyl acetate/absolute ether used in extraction process in step (1), (2) and (3), wherein, wherein the volume ratio of ethyl acetate and absolute ether is 1:1.
7. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol according to any one of claim 1 ~ 4, it is characterized in that, described water-solubility membrane base comprises Pul and shaddock ped polysaccharide, and wherein Pul and shaddock ped polysaccharide compound proportion are 1:3 ~ 3:1; Preferably, Pul and shaddock ped polysaccharide compound proportion are 1:3.
8. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol according to any one of claim 1 ~ 4, it is characterized in that, described plant polyose is shaddock ped polysaccharide; Preferably, described shaddock ped polysaccharide prepares by the following method: shaddock ped is extracted ungrease treatment through supercritical carbon dioxide extraction equipment, then soak first time shaddock ped leaching liquor; Will first time shaddock ped leaching liquor cellulase and pectinase enzymatic hydrolysis, centrifugal, filter; Filtrate is crossed the hollow-fibre membrane that molecular cut off is 100,000 again, collect permeate, obtain shaddock ped extract; Be 40 ~ 80% ethanol alcohol precipitations respectively by shaddock ped extract volume fraction, obtain 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c; 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c are obtained shaddock ped polysaccharide so that the ratio of weight ratio 1:3:2 ~ 3:1:2 is composite; Preferably, 40% alcohol settling polysaccharide a, 60% alcohol settling polysaccharide b, 80% alcohol settling polysaccharide c obtain shaddock ped polysaccharide so that the ratio of weight ratio 1:2:1 is composite.
9. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol according to any one of claim 1 ~ 4, it is characterized in that, the formulation of the described cold fresh-keeping agent for meat of film base compound mangosteen polyphenol is aqua form, and wherein the concentration of each component is: mangosteen shell free state phenol 0.5 ~ 1.5g/L, mangosteen shell esterification state phenol 1.0 ~ 2.0g/L, mangosteen shell are in conjunction with state phenol 0.5 ~ 1.0 g/L, nisin 0.02 ~ 0.07 g/L, sodium hexametaphosphate 3 ~ 6 g/L, water-solubility membrane base 5 ~ 15 g/L.
10. the cold fresh-keeping agent for meat of film base compound mangosteen polyphenol according to claim 9, it is characterized in that, the concentration of each component is: mangosteen shell free state phenol 1.0g/L, mangosteen shell esterification state phenol 1.5g/L, mangosteen shell are in conjunction with state phenol 0.8 g/L, nisin 0.05 g/L, sodium hexametaphosphate 5g/L, water-solubility membrane base 10g/L.
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| CN109172712A (en) * | 2018-10-09 | 2019-01-11 | 昆明理工大学 | The purposes of palm berry extract |
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