CN106580916B - A kind of preparation method of allicin microcapsule - Google Patents
A kind of preparation method of allicin microcapsule Download PDFInfo
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- CN106580916B CN106580916B CN201611135621.6A CN201611135621A CN106580916B CN 106580916 B CN106580916 B CN 106580916B CN 201611135621 A CN201611135621 A CN 201611135621A CN 106580916 B CN106580916 B CN 106580916B
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- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K31/00—Medicinal preparations containing organic active ingredients
- A61K31/21—Esters, e.g. nitroglycerine, selenocyanates
- A61K31/255—Esters, e.g. nitroglycerine, selenocyanates of sulfoxy acids or sulfur analogues thereof
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K9/00—Medicinal preparations characterised by special physical form
- A61K9/48—Preparations in capsules, e.g. of gelatin, of chocolate
- A61K9/50—Microcapsules having a gas, liquid or semi-solid filling; Solid microparticles or pellets surrounded by a distinct coating layer, e.g. coated microspheres, coated drug crystals
- A61K9/5005—Wall or coating material
- A61K9/5021—Organic macromolecular compounds
- A61K9/5036—Polysaccharides, e.g. gums, alginate; Cyclodextrin
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Abstract
The invention belongs to microcapsules technology fields, and in particular to a kind of preparation method of novel allicin microcapsule.Mainly using the allicin in fresh garlic as core material, the amylose of hydrophilic and oleophilic double grading is wall material, at normal temperature squeezes fresh mashed garlic and amylose by extrusion and microcapsules are made.Its main feature is that forming Inclusion Complexes by supermolecular mechanism using the allicin in the hydrophobic interior cavities and garlic of amylose helical structure, allicin molecule can be embedded, novel allicin microcapsule is formed, which overcomes current garlic process and be deodorized the deficiencies of at high cost, allicin structure is easily destroyed, technique is cumbersome or influences garlic flavor by the introducing of other additives.This novel allicin microcapsule volatile sulfur compound caused by tight garlic but also can protect the other effective components and nutritional ingredient of garlic, have biggish alimentary health-care function.
Description
Technical field
The present invention relates to a kind of preparation methods of novel allicin microcapsule, belong to micro-capsule preparation technical field.It can also answer
For medicine, nutriment, health products trade.
Background technique
Allicin (Allicin) is main component in garlic, is a kind of compound containing allyl sulfide, has strong thorn
Swash property, assigns the distinctive acid of garlic.There is allicin has a broad antifungal spectrum antitumor, anti-aging, antimicrobial, raising body to exempt from
Epidemic disease power, the multiple pharmacological effect for preventing cardiovascular and cerebrovascular disease.For a long time, natural spice is directly added into dish tune by people
Taste can neither fully utilize raw material in this way, and bring many inconvenience to consumer, and because of effective component and fragrance matter
Loss, limits it and promotes in the market.In order to improve the bioavilability of garlic and improve bad smell, domestic and foreign scholars' phase
After the preparation method for having studied a variety of allicin microcapsules: such as, Arabic gum and maltodextrin is used to shelter stink for wall material, and
The stability of Arabic gum emulsion is poor, and price is higher, and micro-capsule easily agglomerates, and (old snow peak, Liu Di, Zhang Yongsheng wait the micro- glue of garlic oil
Production technology [J] food and fermentation industries of capsule, 2004,30 (10): 64-67).With Arabic gum, maltodextrin, gelatin, sugarcane
The phenomenon that sugar is compound wall materials, embeds allicin, and micro-capsule is made using spray drying technology, and particle has agglomeration, glues wall, embedding
Rate is low (He Ronghai, Ma Haile spray drying process produce allicin microcapsule [J] food industry, 2004,3:7-8).Microencapsulation
Allinnase such as micro-wave vacuum method is sheltered, Li et al. carries out embedding twice to garlic powder using improvement fluidization and sustained release is made
Micro-capsule, the method bioavilability is high, covers offending smell, protects garlic powder effective component, but technique requires high, operating condition
Harshness (Li Y, Xu S Y, Sun D W.Preparation of garlic powder with high allicin
content by using combined microwave-vacuum and vacuum drying as well as
Microencapsulation [J] .Journal of Food Engineering, 2007,83 (1): 76-83).
Microcapsules granulating technique is by the embedding of solid, liquid or gaseous matter, seals up for safekeeping in a kind of miniature glue as one kind
The technology of solia particle product can protect guest molecule in this way, be allowed to completely cut off with extraneous unfavorable environment, reach maximum limit
Degree ground keeps original color, smell and taste, performance and bioactivity, prevents the destruction and loss of nutritional ingredient.Microcapsules technology is substantially
The quality of a kind of packing technique, effect is closely related with the selection of wall material, and the characteristic of wall material determines microencapsulation product
Performance is such as: slow release, mobility, dissolubility, while having an effect on microencapsulation production technology, and therefore, the selection of wall material is to influence
Microencapsulation primarily solves the problems, such as.
Amylose can interact to form complex compound with hydrophobic ligand, and to the area requirement of embedding ligand sizes
The single coil configuration of width, amylose can induce hydrophobic guest molecules, form complex compound.Since amylose is in ative starch
On the basis of formed spiraled cavity structure, the double grading of external hydrophilicity with internal drainage, to have excellent film forming
And emulsibility, microcapsules can be formed from different hydrophobic molecules.Therefore squeezed under the action of mechanical force, under room temperature,
It is not required to add other substances, allicin can enter in starch spiraled cavity, form novel allicin microcapsule, and microencapsulation is made
Powder spice had not only been able to maintain the effective component and original local flavor of garlic in this way, but also can be rotten to avoid going rotten, easy to use,
Volume, which is greatly reduced, simultaneously carrys out huge interests to commercial transportation storage tape, and extrusion has energy-saving safety, low consumption, yield height etc.
A little.
Summary of the invention
For the present invention using amylose as wall material, allicin is core material, is prepared under normal temperature condition using extrusion novel big
Allicin microcapsules measure the content of allicin in micro-capsule according to HPLC method, calculate embedding rate, are that examination refers to embedding rate and yield
Mark, and physical characterization is carried out to its structure, verify the formation of microcapsules.It is intended to embed the stink of garlic, prevents the effective of garlic
Ingredient and nutrient loss extend the validity period of product.
Technical solution of the present invention
A kind of preparation method of novel allicin microcapsule, feature mainly comprise the steps that
(1) by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
(2) it controls amylose and uniform wall material is made in the mass ratio of pure water；
(3) by mashed garlic and wall material, mixture is made according to certain mass ratio；
(4) mixture obtained by step (3) is sufficiently squeezed to required time using extruder, and is obtained after being dried at room temperature for
Novel allicin microcapsule.
Beneficial effects of the present invention:
(1) a kind of novel allicin microcapsule preparation method, under room temperature, by extrusion by the allicin in fresh garlic
Entered in the spiraled cavity of amylose by supermolecular mechanism, protect allicin structure and its fresh garlic nutrition at
Point.
(2) in preparation process in addition to using water, other any solvents are not used.The system of this novel allicin microcapsule
Preparation Method is remained without organic solvent.
(3) preparation process is easy, and yield is high, at low cost.
Detailed description of the invention
The preparation technology parameter of the novel allicin microcapsule of Fig. 1 screens
A. amylose/mashed garlic mass ratio (g/g)；B. amylose/water mass ratio (g/g)；C. extrusion time (h)
The high phase liquid-phase chromatographic analysis of the novel allicin microcapsule of Fig. 2
A. negative controls solution；B. allicin standard solution；C. the sample solution of allicin microcapsule
The X-ray diffractogram of the novel allicin microcapsule of Fig. 3
A. amylose；B. allicin microcapsule (amylose and garlic mass ratio 2: 2)；C. allicin microcapsule is (straight
Chain starch and garlic 6: 2)；D. allicin microcapsule (amylose and garlic 4: 2)
The gas chromatography-mass spectrography chemical composition analysis of the novel allicin microcapsule of Fig. 4
A. fresh garlic:
1.Dimethyl trisulfide；2. 1,3-Dithiane；3. 3-Vinyl-1,2-dithiocyclohex-
5-ene；4. 3-Vinyl-1,3-dithiine；5.Diallyl disulphide；6. 1,2-Dithiolane；
7.Diallyl sulfide；8.Methyl propyl disulfide；9.Diallyl trisulfide；10.Diallyl
tetrasulfide；11.Allyl methyl trisulfide
B. allicin microcapsule:
1.Dimethyl trisulfide；2. 1,3-Dithiane；3. 3-Vinyl-1,2-dithiocyclohex-
5-ene；4. 3-Vinyl-1,3-dithiine；5.Diallyl disulphide；6. 1,2-Dithiolane；
7.Diallyl sulfide；8.Methyl propyl disulfide；9.Diallyl trisulfide；10.Diallyl
tetrasulfide；11.Allyl methyl trisulfide
Specific embodiment
Embodiment 1
A. by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
B. it controls amylose and uniform wall material is made in the mass ratio 4: 5 of pure water；
C. by mashed garlic and wall material, mixture is made according to mass ratio 2: 4；
D. above-mentioned gained mixture is sufficiently squeezed to 1h using extruder, it is micro- that novel allicin is obtained after being dried at room temperature for
Capsule.
Yield is 60.25%, embedding rate 51.55%.
Embodiment 2
A. by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
B. it controls amylose and uniform wall material is made in the mass ratio 4: 4 of pure water；
C. by mashed garlic and wall material, mixture is made according to mass ratio 2: 4；
D. above-mentioned gained mixture is sufficiently squeezed to 4h using extruder, it is micro- that novel allicin is obtained after being dried at room temperature for
Capsule.
Yield is 91.94%, embedding rate 90.63%.
Embodiment 3
A. by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
B. it controls amylose and uniform wall material is made in the mass ratio 3: 4 of pure water；
C. by mashed garlic and wall material, mixture is made according to mass ratio 2: 4；
D. above-mentioned gained mixture is sufficiently squeezed to 3h using extruder, it is micro- that novel allicin is obtained after being dried at room temperature for
Capsule.
Yield 70.25%, embedding rate 50.11%.
Embodiment 4
A. by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
B. it controls amylose and uniform wall material is made in the mass ratio 1: 4 of pure water；
C. by mashed garlic and wall material, mixture is made according to mass ratio 2: 4；
D. above-mentioned gained mixture is sufficiently squeezed to 2h using extruder, it is micro- that novel allicin is obtained after being dried at room temperature for
Capsule.
Yield is 60.20%, embedding rate 45.22%.
Embodiment 5
A. by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
B. it controls amylose and uniform wall material is made in the mass ratio 4: 4 of pure water；
C. by mashed garlic and wall material, mixture is made according to mass ratio 2: 2；
D. above-mentioned gained mixture is sufficiently squeezed to 4h using extruder, it is micro- that novel allicin is obtained after being dried at room temperature for
Capsule.
Yield is 60.27%, embedding rate 58.83%.
Embodiment 6
A. by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
B. it controls amylose and uniform wall material is made in the mass ratio 4: 4 of pure water；
C. by mashed garlic and wall material, mixture is made according to mass ratio 2: 3；
D. above-mentioned gained mixture is sufficiently squeezed to 4h using extruder, it is micro- that novel allicin is obtained after being dried at room temperature for
Capsule.
Yield is 75.60%, embedding rate 47.36%.
Embodiment 7
A. by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
B. it controls amylose and uniform wall material is made in the mass ratio 4: 5 of pure water；
C. by mashed garlic and wall material, mixture is made according to mass ratio 2: 5；
D. above-mentioned gained mixture is sufficiently squeezed to 4h using extruder, it is micro- that novel allicin is obtained after being dried at room temperature for
Capsule.
Yield is 70.30%, embedding rate 48.69%.
Embodiment 8
A. by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
B. it controls amylose and uniform wall material is made in the mass ratio 4: 4 of pure water；
C. by mashed garlic and wall material, mixture is made according to mass ratio 2: 6；
D. above-mentioned gained mixture is sufficiently squeezed to 4h using extruder, it is micro- that novel allicin is obtained after being dried at room temperature for
Capsule.
Yield is 62.50%, embedding rate 48.90%
Embodiment 9
A. by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
B. it controls amylose and uniform wall material is made in the mass ratio 4: 4 of pure water；
C. by mashed garlic and wall material, mixture is made according to mass ratio 2: 5；
D. above-mentioned gained mixture is sufficiently squeezed to 3h using extruder, it is micro- that novel allicin is obtained after being dried at room temperature for
Capsule.
Yield is 72.50%, embedding rate 58.35%.
Product prepared by the present invention is passed through into the screening (Fig. 1) of novel allicin microcapsule preparation technology parameter, novel big
The high phase liquid-phase chromatographic analysis (Fig. 2) of allicin microcapsules, the X-ray diffractogram (Fig. 3) of novel allicin microcapsule, novel garlic
Gas chromatography-mass spectrography chemical composition analysis (Fig. 4) result of plain microcapsules proves the formation of novel allicin microcapsule.
Claims (1)
1. a kind of preparation method of allicin microcapsule, feature mainly comprise the steps that
(1) by fresh garlic, peeling is cleaned, is crushed to mashed garlic；
(2) it controls amylose and uniform wall material is made in the mass ratio of pure water；
(3) by mashed garlic and wall material, mixture is made according to certain mass ratio；
(4) mixture obtained by step (3) is sufficiently squeezed to required time using extruder, and obtains garlic after being dried at room temperature for
Plain microcapsules；
The mass ratio 2: 1~6: 5 of step (2) amylose and pure water；Step (3) is described, the quality of mashed garlic and wall material
It is 2: 2~2: 6 than range, the range of extrusion time needed for gained mixture is 1~4h；Step (4) is made that allicin is micro-
The core material of capsule is the allicin in fresh garlic.
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Families Citing this family (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107594406A (en) * | 2017-09-14 | 2018-01-19 | 天津科技大学 | A kind of method of allicin in embedding in situ fresh garlic using starch |
| CN108244645A (en) * | 2018-01-15 | 2018-07-06 | 沈阳师范大学 | The preparation method of little particle amylose-DHA/ resveratrol inclusion compounds |
| CN108244626A (en) * | 2018-01-15 | 2018-07-06 | 沈阳师范大学 | A kind of method that A types crystalline texture starch embedding resveratrol and L- α-phosphatidyl choline prepare microcapsules |
| CN108967988A (en) * | 2018-06-20 | 2018-12-11 | 漯河双汇生物工程技术有限公司 | A kind of microcapsules garlic flavoring and preparation method thereof |
| CN110506885A (en) * | 2019-09-16 | 2019-11-29 | 天津科技大学 | The self-assembly that allicin is formed in starch and garlic and its application as plant bacteriostatic agent |
| CN112655855B (en) * | 2020-11-23 | 2022-04-08 | 国投中鲁果汁股份有限公司 | Laba garlic lactic acid beverage |
| CN114732931A (en) * | 2022-05-06 | 2022-07-12 | 广州阜耀生物科技有限公司 | Preparation method of agilawood microcapsule sustained-release granules |
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| CN1633999A (en) * | 2004-11-19 | 2005-07-06 | 中国海洋大学 | Allicin microcapsule and its preparation method |
| CN102687797A (en) * | 2012-06-13 | 2012-09-26 | 郑州峰源生物技术有限公司 | Micro-capsule coating method of natural garlic powder |
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| CN103242961A (en) * | 2013-05-16 | 2013-08-14 | 陕西科技大学 | Sugar-vitrified essential oil capsule prepared based on extrusion method and preparation method thereof |
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| CN1633999A (en) * | 2004-11-19 | 2005-07-06 | 中国海洋大学 | Allicin microcapsule and its preparation method |
| CN102687797A (en) * | 2012-06-13 | 2012-09-26 | 郑州峰源生物技术有限公司 | Micro-capsule coating method of natural garlic powder |
| CN102771618A (en) * | 2012-08-09 | 2012-11-14 | 上海应用技术学院 | Chewing gum containing amylase-menthone microcapsule and method for preparing chewing gum |
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