CN107048393A - A kind of preparation method of microencapsulation natural - Google Patents
A kind of preparation method of microencapsulation natural Download PDFInfo
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- CN107048393A CN107048393A CN201710154739.1A CN201710154739A CN107048393A CN 107048393 A CN107048393 A CN 107048393A CN 201710154739 A CN201710154739 A CN 201710154739A CN 107048393 A CN107048393 A CN 107048393A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 62
- 239000011347 resin Substances 0.000 claims abstract description 39
- 229920005989 resin Polymers 0.000 claims abstract description 39
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 33
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 31
- 238000005238 degreasing Methods 0.000 claims abstract description 27
- 239000000843 powder Substances 0.000 claims abstract description 23
- 239000002250 absorbent Substances 0.000 claims abstract description 20
- 230000002745 absorbent Effects 0.000 claims abstract description 20
- 239000007788 liquid Substances 0.000 claims abstract description 19
- 239000003480 eluent Substances 0.000 claims abstract description 17
- 239000000463 material Substances 0.000 claims abstract description 17
- 239000000287 crude extract Substances 0.000 claims abstract description 16
- 239000012141 concentrate Substances 0.000 claims abstract description 15
- 238000001035 drying Methods 0.000 claims abstract description 15
- 238000010521 absorption reaction Methods 0.000 claims abstract description 14
- 238000000265 homogenisation Methods 0.000 claims abstract description 14
- 238000001179 sorption measurement Methods 0.000 claims abstract description 9
- 238000001694 spray drying Methods 0.000 claims abstract description 8
- 239000000654 additive Substances 0.000 claims abstract description 7
- 230000000996 additive effect Effects 0.000 claims abstract description 7
- 238000010828 elution Methods 0.000 claims abstract description 3
- 235000006708 antioxidants Nutrition 0.000 claims description 28
- 238000000034 method Methods 0.000 claims description 19
- 235000019441 ethanol Nutrition 0.000 claims description 18
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 14
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 12
- CIWBSHSKHKDKBQ-JLAZNSOCSA-N Ascorbic acid Chemical compound OC[C@H](O)[C@H]1OC(=O)C(O)=C1O CIWBSHSKHKDKBQ-JLAZNSOCSA-N 0.000 claims description 10
- WHGYBXFWUBPSRW-FOUAGVGXSA-N beta-cyclodextrin Chemical compound OC[C@H]([C@H]([C@@H]([C@H]1O)O)O[C@H]2O[C@@H]([C@@H](O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O[C@H]3O[C@H](CO)[C@H]([C@@H]([C@H]3O)O)O3)[C@H](O)[C@H]2O)CO)O[C@@H]1O[C@H]1[C@H](O)[C@@H](O)[C@@H]3O[C@@H]1CO WHGYBXFWUBPSRW-FOUAGVGXSA-N 0.000 claims description 9
- 235000010837 Echinocereus enneacanthus subsp brevispinus Nutrition 0.000 claims description 7
- 235000006850 Echinocereus enneacanthus var dubius Nutrition 0.000 claims description 7
- 230000008569 process Effects 0.000 claims description 7
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 6
- 238000004821 distillation Methods 0.000 claims description 6
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- 235000013399 edible fruits Nutrition 0.000 claims description 6
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- 238000005406 washing Methods 0.000 claims description 6
- IIZPXYDJLKNOIY-JXPKJXOSSA-N 1-palmitoyl-2-arachidonoyl-sn-glycero-3-phosphocholine Chemical compound CCCCCCCCCCCCCCCC(=O)OC[C@H](COP([O-])(=O)OCC[N+](C)(C)C)OC(=O)CCC\C=C/C\C=C/C\C=C/C\C=C/CCCCC IIZPXYDJLKNOIY-JXPKJXOSSA-N 0.000 claims description 5
- ZZZCUOFIHGPKAK-UHFFFAOYSA-N D-erythro-ascorbic acid Natural products OCC1OC(=O)C(O)=C1O ZZZCUOFIHGPKAK-UHFFFAOYSA-N 0.000 claims description 5
- 229930003268 Vitamin C Natural products 0.000 claims description 5
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- 229940067606 lecithin Drugs 0.000 claims description 5
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- 235000015165 citric acid Nutrition 0.000 claims description 2
- 238000003795 desorption Methods 0.000 claims description 2
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- 235000011949 flavones Nutrition 0.000 description 5
- 239000007921 spray Substances 0.000 description 5
- HIXDQWDOVZUNNA-UHFFFAOYSA-N 2-(3,4-dimethoxyphenyl)-5-hydroxy-7-methoxychromen-4-one Chemical compound C=1C(OC)=CC(O)=C(C(C=2)=O)C=1OC=2C1=CC=C(OC)C(OC)=C1 HIXDQWDOVZUNNA-UHFFFAOYSA-N 0.000 description 4
- GAMYVSCDDLXAQW-AOIWZFSPSA-N Thermopsosid Natural products O(C)c1c(O)ccc(C=2Oc3c(c(O)cc(O[C@H]4[C@H](O)[C@@H](O)[C@H](O)[C@H](CO)O4)c3)C(=O)C=2)c1 GAMYVSCDDLXAQW-AOIWZFSPSA-N 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 4
- 239000003814 drug Substances 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N ether Substances CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 4
- 239000003208 petroleum Substances 0.000 description 4
- 238000005292 vacuum distillation Methods 0.000 description 4
- VHBFFQKBGNRLFZ-UHFFFAOYSA-N vitamin p Natural products O1C2=CC=CC=C2C(=O)C=C1C1=CC=CC=C1 VHBFFQKBGNRLFZ-UHFFFAOYSA-N 0.000 description 4
- 241000675108 Citrus tangerina Species 0.000 description 3
- 206010011732 Cyst Diseases 0.000 description 3
- 235000018481 Hylocereus undatus Nutrition 0.000 description 3
- 206010062717 Increased upper airway secretion Diseases 0.000 description 3
- 238000002835 absorbance Methods 0.000 description 3
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- 239000011782 vitamin Substances 0.000 description 3
- 229940088594 vitamin Drugs 0.000 description 3
- 150000003722 vitamin derivatives Chemical class 0.000 description 3
- 235000001759 Citrus maxima Nutrition 0.000 description 2
- 229940123457 Free radical scavenger Drugs 0.000 description 2
- 229930014669 anthocyanidin Natural products 0.000 description 2
- 150000001452 anthocyanidin derivatives Chemical class 0.000 description 2
- 235000008758 anthocyanidins Nutrition 0.000 description 2
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- 239000000284 extract Substances 0.000 description 2
- PSFDQSOCUJVVGF-UHFFFAOYSA-N harman Chemical compound C12=CC=CC=C2NC2=C1C=CN=C2C PSFDQSOCUJVVGF-UHFFFAOYSA-N 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 229910052738 indium Inorganic materials 0.000 description 2
- 238000012856 packing Methods 0.000 description 2
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- 230000003449 preventive effect Effects 0.000 description 2
- 238000000746 purification Methods 0.000 description 2
- 239000002516 radical scavenger Substances 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- CDBYLPFSWZWCQE-UHFFFAOYSA-L sodium carbonate Substances [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 description 2
- 230000002195 synergetic effect Effects 0.000 description 2
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- 102000004190 Enzymes Human genes 0.000 description 1
- 108090000790 Enzymes Proteins 0.000 description 1
- 208000001953 Hypotension Diseases 0.000 description 1
- IMQLKJBTEOYOSI-GPIVLXJGSA-N Inositol-hexakisphosphate Chemical compound OP(O)(=O)O[C@H]1[C@H](OP(O)(O)=O)[C@@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@H](OP(O)(O)=O)[C@@H]1OP(O)(O)=O IMQLKJBTEOYOSI-GPIVLXJGSA-N 0.000 description 1
- 241001465754 Metazoa Species 0.000 description 1
- 206010028980 Neoplasm Diseases 0.000 description 1
- IMQLKJBTEOYOSI-UHFFFAOYSA-N Phytic acid Natural products OP(O)(=O)OC1C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C(OP(O)(O)=O)C1OP(O)(O)=O IMQLKJBTEOYOSI-UHFFFAOYSA-N 0.000 description 1
- 206010035664 Pneumonia Diseases 0.000 description 1
- 206010036590 Premature baby Diseases 0.000 description 1
- 244000088415 Raphanus sativus Species 0.000 description 1
- 235000006140 Raphanus sativus var sativus Nutrition 0.000 description 1
- 241000607479 Yersinia pestis Species 0.000 description 1
- 239000003463 adsorbent Substances 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229930013930 alkaloid Natural products 0.000 description 1
- 150000003797 alkaloid derivatives Chemical class 0.000 description 1
- 230000003712 anti-aging effect Effects 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 230000001139 anti-pruritic effect Effects 0.000 description 1
- 230000003457 anti-vomiting effect Effects 0.000 description 1
- 239000003908 antipruritic agent Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000005119 centrifugation Methods 0.000 description 1
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- 235000020774 essential nutrients Nutrition 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 150000002213 flavones Chemical class 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 235000019261 food antioxidant Nutrition 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000005556 hormone Substances 0.000 description 1
- 229940088597 hormone Drugs 0.000 description 1
- 230000002218 hypoglycaemic effect Effects 0.000 description 1
- 208000021822 hypotensive Diseases 0.000 description 1
- 230000001077 hypotensive effect Effects 0.000 description 1
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- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 230000003902 lesion Effects 0.000 description 1
- 239000002932 luster Substances 0.000 description 1
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- 235000012054 meals Nutrition 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 235000010987 pectin Nutrition 0.000 description 1
- 229920001277 pectin Polymers 0.000 description 1
- 239000001814 pectin Substances 0.000 description 1
- 235000002949 phytic acid Nutrition 0.000 description 1
- 239000000467 phytic acid Substances 0.000 description 1
- 229940068041 phytic acid Drugs 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 150000008442 polyphenolic compounds Chemical class 0.000 description 1
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- DPJRMOMPQZCRJU-UHFFFAOYSA-M thiamine hydrochloride Chemical compound Cl.[Cl-].CC1=C(CCO)SC=[N+]1CC1=CN=C(C)N=C1N DPJRMOMPQZCRJU-UHFFFAOYSA-M 0.000 description 1
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Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
Landscapes
- Medicinal Preparation (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The present invention discloses a kind of preparation method of microencapsulation natural, including step：A, pericarp carried out to dry and crush for the first time, then degreasing, then carry out second of drying obtains degreasing pericarp powder；B, degreasing pericarp powder is placed in ethanol solution W1 carries out microwave treatment, then constant temperature stirring, filtering, obtain crude extract；C, in crude extract macroporous absorbent resin is put into, carry out adsorption treatment, then take out macroporous absorbent resin, carry out elution processing, eluent is concentrated, obtain refined pericarp Antioxidant Concentrate liquid；D, take refined pericarp Antioxidant Concentrate liquid, add additive, obtain natural compositional liquor；F, take the natural compositional liquor, add wall material, homogenization, spray drying are carried out under the conditions of 35~40MPa, product is produced.The present invention can efficiently against traditional handicraft extraction process final products activity it is not high, easily moisture absorption, it is not easy to maintain, transport inconvenience the problem of.
Description
Technical field
The present invention relates to natural field, more particularly to a kind of preparation side of microencapsulation natural
Method.
Background technology
Natural is the thing with antioxidation activity extracted from natural animal and plant body or its metabolin
Matter, the Polyphenols such as extracted from plant, flavone compound, phytic acid etc..The free radical of aging is proposed from Harman in 1956
Since theory, more and more researchs confirm that free radical excessive in body can trigger various lesions such as:Atherosclerosis, the heart
Vascular diseases and tumour etc., and appropriate supplemented with exogenous antioxidant can improve this situation.Therefore, taken with natural
It is the trend of food antioxidant development from now on for synthetized oxidation preventive agent；The natural materials for removing interior free yl are found simultaneously
It is modern medicine, healthcare industry development trend.
Pericarp such as shaddock ped, dried orange peel, pitaya peel etc., contain what is enriched in substantial amounts of natural, especially dried orange peel
Flavone compound, is strong free radical scavenger, and with very strong antioxidation activity, it is rare that pitaya peel contains general plant
Anthocyanidin, but pericarp is but handled often as waste.
Microcapsules refer to a kind of miniature vessel or packing material with polymer wall, powdered（Liquid, gas etc. are become
Dry powder）, reduction volatility（The material for making some readily volatilized becomes difficult to volatilization）, improve material stability（Easily
Oxidation, is clear to light decomposition, the material easily influenceed by temperature or moisture）, taste masking, isolation active component and control release.
Existing extraction natural anti-oxidation agent method cost is higher, less efficient from pericarp, product purity is not high, be difficult to protect
Deposit, there is presently no a kind of method effectively extracted natural from pericarp and be made into microcapsules.
Therefore, prior art has yet to be improved and developed.
The content of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of microencapsulation natural
Preparation method, it is intended to solve to extract that natural anti-oxidation agent method cost is higher, less efficient, product from pericarp in the prior art
Purity is high, it is not easy to maintain the problem of.
Technical scheme is as follows：
A kind of preparation method of microencapsulation natural, wherein, including step：
A, pericarp carried out to dry and crush for the first time, then carry out degreasing, then carry out second of drying, obtain degreasing fruit peel powder
End；
B, the degreasing pericarp powder is placed in ethanol solution W1 carries out microwave treatment, then constant temperature is stirred, and is refiltered, is obtained
Crude extract；
C, the crude extract put into macroporous absorbent resin, carry out adsorption treatment, the macroporous absorption is taken out after the completion of absorption
Resin, and the macroporous absorbent resin is eluted, eluent is obtained, the eluent is concentrated, refined fruit is obtained
Skin Antioxidant Concentrate liquid；
D, take the refined pericarp Antioxidant Concentrate liquid, add additive, obtain natural compositional liquor；
F, take the natural compositional liquor, add wall material, homogenization, Ran Houjin are carried out under the conditions of 35~40MPa
Row spray drying, produces microencapsulation natural.
A kind of preparation method of microencapsulation natural, wherein, the pericarp is dried orange peel, pomelo peel, dragon fruit
One or more in skin.
A kind of preparation method of microencapsulation natural, wherein, the microwave treatment power is 160w ~ 800w,
Time is 60s ~ 130s.
A kind of preparation method of microencapsulation natural, wherein, before the step C, macroporous absorbent resin is entered
Row is pre-processed, and the pretreatment mode is：
Macroporous absorbent resin absolute ethyl alcohol is fully soaked, distilled water, NaCl solution and Na are then used successively2CO3Solution is rushed
Wash, finally with distillation water washing.
A kind of preparation method of microencapsulation natural, wherein, the macroporous absorbent resin be S-8, AB-8,
One kind in NKA-9, D3520, X-5 resin.
A kind of preparation method of microencapsulation natural, wherein, the elution process in the step C is specially：
Macroporous absorbent resin after the completion of absorption is taken out, is placed in ethanol solution W2, then vibrates, make antioxidant from resin
Upper desorption, obtains eluent.
A kind of preparation method of microencapsulation natural, wherein, contain in the ethanol solution W2 and account for W2 volumes
Fraction is 0.1% ~ 0.5% hydrochloric acid.
A kind of preparation method of microencapsulation natural, wherein, additive in the step D is lecithin,
One or more in vitamin C, citric acid.
A kind of preparation method of microencapsulation natural, wherein, wall material in the step F is beta-schardinger dextrin,
One or more in beta-cyclodextrin derivative.
A kind of preparation method of microencapsulation natural, wherein, the process conditions of the spray drying are：Charging
40 DEG C ~ 60 DEG C of temperature, 160 DEG C~180 DEG C of EAT, 50 DEG C ~ 70 DEG C of leaving air temp.
Beneficial effect：The side that the present invention is combined by using microwave synergistic extraction technique and large aperture resin purification technique
Method, can efficiently against traditional handicraft extraction process final products activity it is not high, easily moisture absorption, it is not easy to maintain, transport and store up
The problem of hiding inconvenience, and use present invention process to extract, the purity of antioxidant composition is not only increased, unit product is improved
Antioxidation activity, and final products are difficult moisture absorption, it is easy to preservation.
Brief description of the drawings
Fig. 1 is the flow chart of the preparation method preferred embodiment of microencapsulation natural of the present invention.
Embodiment
The present invention provides a kind of preparation method of microencapsulation natural, to make the purpose of the present invention, technical side
Case and effect are clearer, clear and definite, and the present invention is described in more detail below.It should be appreciated that specific reality described herein
Example is applied only to explain the present invention, is not intended to limit the present invention.
A kind of preparation method of microencapsulation natural, as shown in figure 1, including step：
S1, pericarp carried out to dry and crush for the first time, then carry out degreasing, then carry out second of drying, obtain degreasing pericarp
Powder；
S2, the degreasing pericarp powder is placed in ethanol solution W1 carries out microwave treatment, then constant temperature is stirred, and is refiltered, is obtained
To crude extract；
S3, the crude extract put into macroporous absorbent resin, carry out adsorption treatment, the macroporous absorption is taken out after the completion of absorption
Resin, and the macroporous absorbent resin is eluted, eluent is obtained, the eluent is concentrated, refined fruit is obtained
Skin Antioxidant Concentrate liquid；
S4, take the refined pericarp Antioxidant Concentrate liquid, add additive, obtain natural compositional liquor；
S5, take the natural compositional liquor, add wall material, homogenization, Ran Houjin are carried out under the conditions of 35~40MPa
Row spray drying, produces microencapsulation natural.
Specifically, the pericarp is the one or more in dried orange peel, pomelo peel, pitaya peel.
Prematurity or maturescent dry outside rind of the sleeve skin for swab, one kind of Chinese medicine Exocarpium Citri Grandis are wide with qi-regulating
In, the effects such as eliminating dampness and eliminating phlegm.Sleeve skin accounts for 1/3rd of swab quality, and some are even up to 2/5ths, wherein not only containing
Necessary to the human bodies such as vitamin, moisture, mineral matter outside factor, also containing many physiologically active ingredients, as pectin, essential oil, meals
Fiber, flavones and polysaccharide compound etc. are eaten, these compositions can improve the interior circulation of human body, there are many benefits to human body.In
Medical knowledge opinion sleeve leatherware have treatment infantile pneumonia, pernio, regulating qi-flowing for eliminating phlegm and it is antipruritic the effects such as.Modern medicine study shows, takes out skin
Extract also has anti-oxidant, antimicrobial, anticancer, suppression enzyme, anti-aging, hypoglycemic, hypotensive and prevention of arterial atherosis
Isoreactivity.
Dried orange peel has promoting the circulation of qi invigorating the spleen, anti-vomiting, eliminating dampness and eliminating phlegm effect, contains abundant flavone compound, flavonoids
Compound is strong free radical scavenger, with very strong antioxidation activity.In addition, also including a small amount of alkaloid in dried orange peel, class is recklessly
The material such as radish element and vitamin C.In dried orange peel also containing a variety of human life essential nutrient elements such as:K、Ca、Na、Mg、Li、
Fe, Zn, Mn etc..
Dragon fruit pericarp also contains substantial amounts of flavone compound, and typically the rare anthocyanidin of plant, vegetalitas are white
Albumen and abundant vitamin and water-soluble dietary fiber., can be without using any agriculture because pest and disease damage seldom occurs in dragon fruit
Medicine and hormone, belong to environmental protection fruit and have extensive development space.
In the step S1, first pericarp is cleaned and dried, is subsequently placed in 40 ~ 65 DEG C of baking oven and dries 4 ~ 6h, to remove
Wherein unnecessary moisture, then dried pericarp is crushed, cross 40 ~ 60 mesh sieves using pulverizer, obtains pericarp powder, and will
Pericarp powder after sieving carries out ungrease treatment, more preferably, and ungrease treatment is carried out to pericarp powder using petroleum ether immersion, and will
Enter the pericarp powder drying of ungrease treatment, that is, obtain degreasing pericarp powder.
It is preferred that before clean pericarp is put into baking oven, pericarp is shredded, to accelerate the removal of moisture.
Further, in the step S2, degreasing pericarp powder is placed in the ethanol solution W1 that volume fraction is 55% ~ 75%
In, microwave treatment is carried out, then constant temperature is stirred, and is refiltered, is obtained crude extract.
It is preferred that degreasing pericarp powder and ethanol solution W1 mass volume ratio are 1:3~1:4（g：mL）, at the microwave
Reason power is 160w ~ 800w, the time be 60s ~ 130s, on this condition, the antioxidant effect of extracting of extract solution it is further preferred that.
Microwave abstracting can effectively protect active ingredient in plant, have higher selectivity, extraction speed to extract
Degree is fast, shortens the production time, and avoids thermal decomposition caused by long-time heating, active ingredient is exempted from destruction, reduction
Solvent consumption and waste yield, meet " green " environmental protection concept, improve extraction of substance purity, products obtained therefrom quality waits well special
Point.
Further, in the step S3, the crude extract obtained in step S2 is inhaled using macroporous absorbent resin
Attached processing, the natural in crude extract is adsorbed in the macroporous absorbent resin, by the macropore after the completion of absorption
Polymeric adsorbent takes out, and is placed in ethanol solution W2, then vibrates, antioxidant is desorbed from resin, obtains eluent, then
Concentration is carried out to eluent using vacuum distillation concentration method, that is, obtains refined pericarp Antioxidant Concentrate liquid.
The macroporous absorbent resin is one kind in S-8, AB-8, NKA-9, D3520, X-5 resin, it is preferred that using S-8
Resin, when adsorption time is up to 150 min, adsorption rate is up to 81.9%.
It is preferred that the volume fraction of the ethanol solution W2 is 20% ~ 80%, excessive concentration or too low is all unfavorable for antioxygen
Agent is desorbed, more preferably, and containing the hydrochloric acid that W2 volume fractions are 0.1% ~ 0.5% is accounted in the ethanol solution W2, antioxidant is returned
Yield is up to 93.4%, and cycles of concentration reaches 17 times, not only reduces energy consumption, while avoiding anti-oxidant during being concentrated under reduced pressure
The degraded and denaturation of agent.
It is preferred that before the step S3, being pre-processed to macroporous absorbent resin, the pretreatment mode is：
Macroporous absorbent resin absolute ethyl alcohol is fully soaked, distilled water, NaCl solution and Na are then used successively2CO3Solution is rushed
Wash, finally with distillation water washing.
It is preferred that the additive in the step S4 is the one or more in lecithin, vitamin C, citric acid.
In the step S5, carrying out homogenization to the natural for adding wall material can make emulsion uniform and stable,
It is easy to spray drying, and homogenization pressure has a great impact to stability, it is preferred that homogenization pressure is 35~40 MPa, works as pressure
When power is less than 40MPa, the stability of emulsion is improved with the increase of homogenization pressure；When pressure is more than 40 MPa, emulsion
Stability change is not obvious.More preferably, under the conditions of 35~40MPa, the natural for adding wall material is carried out equal twice
Matter processing, the stability of emulsion it is further preferred that.
It is preferred that the wall material in the step S5 is the one or more in beta-schardinger dextrin, beta-cyclodextrin derivative, gained
Microencapsulation antioxidant compositional liquor water solubility is greatly improved, and to the stability of heat, light, preservative etc. also very big improvement.
It is preferred that the process conditions of the spray drying in the step S5 are：40 DEG C of feeding temperature ~ 60 DEG C, EAT
160 DEG C~180 DEG C, 50 DEG C ~ 70 DEG C of leaving air temp.
This experiment uses RGW01 drying machine with centrifugal spray, and main technologic parameters are：EAT, leaving air temp, centrifugation speed
Degree and feeding temperature etc..Stability of these technological parameters for the embedding rate of microencapsulated products, granular size and product
There is large effect.
EAT has influence on the rate of drying and drying capacity of microcapsules, is related to the grain structure of product, moisture and contains
Amount and stability.EAT is proper at 160~180 DEG C, during less than 160 DEG C, and product moisture content is big, and mobility is not
It is good, wall easy to stick；EAT is too high, and moisture dissipation speed is fast, and cyst wall surface produces " pitting ", while also resulting in wall material
Film forming is reduced, and influences the embedding effect of product.
Leaving air temp has influence on the drying time of product, has larger shadow for the cyst wall structure and moisture of microcapsules
Ring.In the present invention, leaving air temp is arranged on 50 DEG C ~ 70 DEG C, and leaving air temp is high, is conducive to the complete fine and close cyst wall knot of product formation
Structure, can also make the moisture of product reduces, and is conducive to improving the effect being spray-dried.But temperature is too high also result in product excessively by
Heat and ftracture, the embedding rates of microcapsules is reduced.
Feeding temperature has influence on the mobility of feed liquid, the difficulty or ease of spray process and product viscosity size etc..Properly increase into
Material temperature degree, can reduce the viscosity of charging emulsion, be conducive to emulsion droplet to be atomized, while the concentration of perverse liquid can also be improved.Charging
Temperature can not be too high, and the antioxidant compositional liquor of poor heat resistance otherwise can be caused to decompose.In the present invention, feeding temperature is 40 DEG C
~60℃。
The water solubility of microencapsulation natural is greatly increased compared with natural, and lysate lovely luster,
It is transparent, without precipitation, light resistance preferably, without discolouration phenomena, under conditions of 100 DEG C, inhale within two months by the antioxidant of microencapsulation
The slip of luminosity is only 0.7%, and the slip of the antioxidant compositional liquor absorbance of non-microcapsules is 12.3%, antioxidant
Compositional liquor is after microencapsulation, and its heat resistance has obvious improvement.Meanwhile, in the environment of pH is 1 ~ 6, with acidity increasing
By force, the absorbance of microencapsulation natural is in downward trend, but the percentage very little reduced, and only 4.2%, and
The rate of change of non-microencapsulation antioxidant compositional liquor absorbance is 80% or so, and antioxidant compositional liquor is resistance to after microencapsulation
Acidity is remarkably reinforced.
The present invention is further explained below by embodiment.
Embodiment 1
Dried orange peel is put at baking oven, 65 DEG C and dries 4h, is crushed, 40 mesh sieves, petroleum ether soak degreasing, by the tangerine peel powder after degreasing are crossed
End drying, obtains degreasing Dried Tangerine Peel, takes 10g degreasings Dried Tangerine Peel to add in the ethanol solution that 300mL volume fractions are 55%,
Radiation treatment 60s, is then filtered under 160w microwave power, obtains crude extract, then puts into S-8 in the crude extract
Resin（The S-8 resins are fully soaked with absolute ethyl alcohol in advance, and distilled water, NaCl solution and Na are then used successively2CO3Solution is rushed
Wash, finally with distillation water washing）, adsorption treatment is carried out, is then that 0.1%HCl-20% ethanol solutions are washed with volume fraction
It is de-, eluent is obtained, concentration is then carried out to eluent using vacuum distillation concentration method, that is, obtains refined pericarp anti-oxidant
Agent concentrate, adds a certain amount of lecithin and vitamin in refined pericarp Antioxidant Concentrate liquid, stirs, add
Beta-schardinger dextrin, twice homogenization processing is then carried out under 35 MPa homogenization pressure, natural compositional liquor is obtained, finally
Using RGW01 drying machine with centrifugal spray, under conditions of 40 DEG C of feeding temperature, 160 DEG C of EAT, 50 DEG C of leaving air temp, enter
Row spray drying, produces microencapsulation natural.
Embodiment 2
Pomelo peel is put at baking oven, 40 DEG C and dries 4h, is crushed, 60 mesh sieves, petroleum ether soak degreasing, by the shaddock after degreasing are crossed
Skin powder is dried, and obtains degreasing pomelo peel powder, takes 10g degreasing pomelo peels powder to add the ethanol that 400mL volume fractions are 75%
In solution, radiation treatment 130s, is then filtered under 800w microwave power, obtains crude extract, then in the coarse extraction
Liquid puts into AB-8 resins（The AB-8 resins are fully soaked with absolute ethyl alcohol in advance, then successively with distilled water, NaCl solution and
Na2CO3Solution is rinsed, finally with distillation water washing）, adsorption treatment is carried out, is then 0.5%HCl-80% ethanol with volume fraction
Solution is eluted, and obtains eluent, is then carried out concentration to eluent using vacuum distillation concentration method, that is, is refined
Pericarp Antioxidant Concentrate liquid, a certain amount of vitamin C and citric acid are added in refined pericarp Antioxidant Concentrate liquid, stirring
Uniformly, beta-cyclodextrin derivative is added, twice homogenization processing is then carried out under 40 MPa homogenization pressure, is naturally resisted
Oxidant compositional liquor, finally using RGW01 drying machine with centrifugal spray, in 60 DEG C of feeding temperature, 180 DEG C of EAT, goes out wind-warm syndrome
Under conditions of 70 DEG C of degree, it is spray-dried, produces microencapsulation natural.
Embodiment 3
Pitaya peel is put at baking oven, 50 DEG C and dries 6h, is crushed, 40 mesh sieves, petroleum ether soak degreasing, by the fire after degreasing are crossed
Imperial pericarp powder drying, obtains degreasing pitaya peel powder, takes 10g degreasing pitaya peels powder to add 400mL volume fractions and is
In 73% ethanol solution, radiation treatment 80s, is then filtered under 640w microwave power, obtains crude extract, then in institute
State crude extract input S-8 resins（The S-8 resins are fully soaked with absolute ethyl alcohol in advance, and distilled water, NaCl are then used successively
Solution and Na2CO3Solution is rinsed, finally with distillation water washing）, adsorption treatment is carried out, is then 0.2%HCl- with volume fraction
40% ethanol solution is eluted, and obtains eluent, then carries out concentration to eluent using vacuum distillation concentration method, i.e.,
Refined pericarp Antioxidant Concentrate liquid is obtained, a certain amount of lecithin, dimension life are added in refined pericarp Antioxidant Concentrate liquid
Plain C and citric acid, are stirred, and add beta-schardinger dextrin, and twice homogenization processing is then carried out under 35 MPa homogenization pressure,
Natural compositional liquor is obtained, finally using RGW01 drying machine with centrifugal spray, in 50 DEG C of feeding temperature, EAT 170
DEG C, under conditions of 60 DEG C of leaving air temp, be spray-dried, produce microencapsulation natural.
The method that the present invention is combined by using microwave synergistic extraction technique and large aperture resin purification technique, can be effective
Ground overcomes the final products easily moisture absorption of traditional handicraft extraction process, not easy to maintain, is made troubles for Tibetan of transporting and hurry, and uses
Present invention process is extracted, and is not only increased the purity of antioxidant composition, is improved unit product antioxidation activity, and finally
Product is difficult moisture absorption, it is easy to preservation.
The color of this product can be packed using paper bag packing and paper web to be light brown, its antioxidation activity with dosage people
Work synthetized oxidation preventive agent quite, but in the absence of potential safety hazard, can be widely applied to the neck such as food additives, health products and cosmetics
Domain.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can
To be improved or converted according to the above description, all these modifications and variations should all belong to the guarantor of appended claims of the present invention
Protect scope.
Claims (10)
1. a kind of preparation method of microencapsulation natural, it is characterised in that including step：
A, pericarp carried out to dry and crush for the first time, then carry out degreasing, then carry out second of drying, obtain degreasing fruit peel powder
End；
B, the degreasing pericarp powder is placed in ethanol solution W1 carries out microwave treatment, then constant temperature is stirred, and is refiltered, is obtained
Crude extract；
C, the crude extract put into macroporous absorbent resin, carry out adsorption treatment, the macroporous absorption is taken out after the completion of absorption
Resin, and the macroporous absorbent resin is eluted, eluent is obtained, the eluent is concentrated, refined fruit is obtained
Skin Antioxidant Concentrate liquid；
D, take the refined pericarp Antioxidant Concentrate liquid, add additive, obtain natural compositional liquor；
F, take the natural compositional liquor, add wall material, homogenization, Ran Houjin are carried out under the conditions of 35~40MPa
Row spray drying, produces microencapsulation natural.
2. the preparation method of microencapsulation natural according to claim 1, it is characterised in that the pericarp is
One or more in dried orange peel, pomelo peel, pitaya peel.
3. the preparation method of microencapsulation natural according to claim 1, it is characterised in that at the microwave
Reason power is 160w ~ 800w, and the time is 60s ~ 130s.
4. the preparation method of microencapsulation natural according to claim 1, it is characterised in that the step C
Before, macroporous absorbent resin is pre-processed, the pretreatment mode is：
Macroporous absorbent resin absolute ethyl alcohol is fully soaked, distilled water, NaCl solution and Na are then used successively2CO3Solution is rushed
Wash, finally with distillation water washing.
5. the preparation method of microencapsulation natural according to claim 1, it is characterised in that the macropore is inhaled
Attached resin is one kind in S-8, AB-8, NKA-9, D3520, X-5 resin.
6. the preparation method of microencapsulation natural according to claim 1, it is characterised in that the step C
In elution process be specially：
Macroporous absorbent resin after the completion of absorption is taken out, is placed in ethanol solution W2, then vibrates, make antioxidant from resin
Upper desorption, obtains eluent.
7. the preparation method of microencapsulation natural according to claim 6, it is characterised in that the ethanol is molten
Contain the hydrochloric acid for accounting for that W2 volume fractions are 0.1% ~ 0.5% in liquid W2.
8. the preparation method of microencapsulation natural according to claim 1, it is characterised in that the step D
In additive be lecithin, vitamin C, citric acid in one or more.
9. the preparation method of microencapsulation natural according to claim 1, it is characterised in that the step F
In wall material be beta-schardinger dextrin, beta-cyclodextrin derivative in one or more.
10. the preparation method of microencapsulation natural according to claim 9, it is characterised in that the spraying
Dry process conditions are：40 DEG C ~ 60 DEG C of feeding temperature, 160 DEG C~180 DEG C of EAT, 50 DEG C ~ 70 DEG C of leaving air temp.
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| CN111084373A (en) * | 2019-12-20 | 2020-05-01 | 吉林省桦树茸国际健康产业集团有限公司 | Extraction and microencapsulation of antioxidant component in Inonotus obliquus and application of antioxidant component in biscuit |
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Application publication date: 20170818 |