CN1163155C - Productive technology for microcapsule plant extract - Google Patents
Productive technology for microcapsule plant extract Download PDFInfo
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- CN1163155C CN1163155C CNB991159047A CN99115904A CN1163155C CN 1163155 C CN1163155 C CN 1163155C CN B991159047 A CNB991159047 A CN B991159047A CN 99115904 A CN99115904 A CN 99115904A CN 1163155 C CN1163155 C CN 1163155C
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Abstract
The present invention relates to a production technique for extracting plant physiological active constituents and making a microcapsule product. The present invention comprises the procedures of microwave solvent extraction at low temperature, distillation and concentration under negative pressure and at low temperature, maillard reaction of extraction residue, extractant emulsification and homogenization, supersonic spray drying under negative pressure and at low temperature, etc. The microcapsule molding of the technique does not use wall material, extractant moves by self and is shaped in a supersonic spray process, and the extractant is instantaneously dried under negative pressure and at low temperature. The product which is produced by the present invention has the characteristics of complete and thorough plant extract extraction, ideal embedding, good dissolvability and long retention period.
Description
The present invention relates to a kind of production method of the physiologically active of plant composition being extracted and makes microcapsule product.It is specially adapted to the refining of natural plants such as spice, Chinese herbal medicine, food and preserves.
In prior art, Chinese patent 96117699 discloses a kind of " production technology of microcapsule of fragrant and pungent oil extract ", and main technical process is: earlier with raw material pulverizing, extract plant oil resin with the solvent diacolation then under room temperature or low temperature; Make core with the plant oil resin of extraction gained again, edible glue is made the wall material, carry out the emulsification packing, thereby form wet microcapsules emulsion, wherein used edible glue is that two or more mixes in proportion in Arabic gum, maltodextrin, yellow source glue and the soluble starch; At last emulsion is pumped into and carry out spray-drying in the spray dryer, get microcapsule product, dry EAT is 80～100 ℃, and leaving air temp is 40～60 ℃.This technology thinks that it has solved three problems: the first, under room temperature or low temperature, extract, and reduce the loss of volatile ingredient in the extraction process; The second, for reducing the cost of wall material (Arabic gum), adopt cheap maltodextrin, yellow source glue and soluble starch and Arabic gum to be mixed and made into edible glue in proportion and replace very expensive Arabic gum; The 3rd, control spray dryer baking temperature is avoided high temperature drying to cause the part component to be destroyed and is made disadvantages such as mouthfeel degenerates.
In fact, this patent application solves all not ideal enoughly to above-mentioned three problems.First problem, in room temperature or low temperature (below 50 ℃) extraction down, though can reduce the loss of volatile ingredient, and the physiologically active ingredient of plant be not destroyed (as long as can be not destroyed below 50 ℃), but the also corresponding reduction of dissolution rate makes extraction not thorough, has at least the extraction of 20% active ingredient not come out, causing very big wastage of material, is very disadvantageous to large-scale industrial production.
Above-mentioned second and the 3rd problem is the problem that belongs in the microcapsules technology field, and wherein second problem is still the most realistic problem that faces in the present microcapsules technology field.Because Arabic gum (wall material) has ring shaped molecule structure, form embedding easily, and dissolubility is good,, it is the first-selected material of microcapsule wall material so being praised highly always.But it is too expensive, and consumption is big, therefore, has limited the extensive use of microcapsules technology greatly.If can obtain breaking through on wall material cost, microcapsules technology will obtain application prospect widely at spice, Chinese herbal medicine and field of food.So, reduce the bottleneck difficulty that wall material cost has become this area main attack.Above-mentioned patent application is attempted in this respect, and also there are the development report of this respect " food industry science and technology " 99 years the 2nd phases of magazine (P34) and 99 years the 5th phases (P8), but they all do not have breakthrough progress.In fact, Arabic gum or edible glue are not desirable wall materials, because on their miniature form, their ring shaped molecule structure is actually a kind of network structure, volatile ingredient slowly discharges by network structure easily, and this long preservation to product is disadvantageous.Moreover the dissolubility of domestic edible glue all is not so good as Arabic gum, with it replace or the part replace Arabic gum also can have influence on the instant performance of product.
The 3rd problem also is more scabrous problem in the present microcapsules technology, and above-mentioned patent application is to the EAT of spray dryer and go out temperature and limit, and by limiting straying quatity, reaches dry at low temperatures purpose simultaneously.That is to say that it is to have exchanged low temperature drying for reducing dry generation rate, this exchange is unaccommodated to large-scale production.Moreover it so surpass 50 ℃ probably in the drying, causes the loss of volatile ingredient to not control of the maximum temperature point in the drying machine.In addition, the spray dryer that its adopts is common Highspeedcentrifugingandsprayingdrier, and this also is present this area widespread usage.Its action principle is: by the high speed centrifugation nebulization, make emulsion fully be broken into fine droplet, be dried to microcapsule product then.This spray dryer is to the not effect of formation of microcapsules.
In sum, up to the present, yet there are no a kind of more satisfactory microcapsule plant extract preparation technology and come out.
The objective of the invention is not thoroughly and problem such as the microcapsules moulding process is undesirable at low-temperature extraction in the prior art, a kind of production technology of improved microcapsule plant extract is provided, reaches purposes such as improving the quality of products, reduce production costs, simplify production process.
For achieving the above object, the improved processing step of the present invention is as follows:
One, the extraction of plant oil resin: plant material is put into the microwave abstracting jar carry out the microwave solvent extraction, 35～45 ℃ of extraction temperature, pressure 0.06～0.12MPa, solution after the extraction is sent into concentration tank, vacuumize distillation and concentrate, get plant oil resin or plant extracts, thickening temperature is lower than 50 ℃, vaporized gas is sent into rectifying column in concentrating, and obtains phytovolatilization essential oil and recovered solvent by condensation, separation;
Two, Maillard reaction: will extract 100～120 ℃ of last plant residue heating, be incubated 10～20 minutes, making plant residue is that catalyst at high temperature produces Maillard reaction with residual solvent, the plant heteroaromatic composition that evaporates in the reaction enters rectifying column, obtains Maillard reaction oil by condensation, separation;
Three, mixing of the emulsification of plant oil resin and emulsion or plant extracts and above-mentioned Maillard reaction oil and phytovolatilization essential oil: the standard adding emulsifying agent of in the plant oil resin of extraction gained, press the state food additive, stir, add the Maillard reaction oil and the phytovolatilization essential oil of gained again, stir; Perhaps will extract plant extracts and the phytovolatilization essential oil and the directly mixing of Maillard reaction oil of gained, stir;
Four, homogeneous: the emulsion that mixes or extract mixing liquid are sent in the homogenizer homogeneous under 15～25MPa, obtain emulsion;
Five, supersonic speed spraying negative pressure drying: the emulsion of homogeneous gained sent in the supersonic speed spraying negative pressure drying machine be dried to the plant microcapsule product, the flow velocity of supersonic speed spraying is 340～800 meter per seconds under pressure 0.4～0.7MPa, the tower inner drying is to limit highest temperature zone temperature in the tower, to limit EAT and leaving air temp is auxilliary, be that the highest temperature zone temperature is defined as 40～50 ℃ in the tower, and the negative pressure with 0.02～0.03Mpa is moved in the tower.
By above-mentioned improved technology as can be seen, the present invention has adopted microwave extraction process, make raw material utilize microwave processing at low temperatures and shortening, so not only improve the dissolution rate of extraction but also guaranteed low-temperature extraction, simultaneously, its low-temperature negative-pressure distillation concentration technology can reduce the vapourizing temperature point of solution by negative pressure, and is concentrated fast at low temperatures to guarantee.The Maillard reaction that the present invention adopts can obtain the heterocyclic aromatic compounds in the raw material, makes product have ripe fragrance breath.The supersonic speed spraying negative pressure low temperature drying technology that the present invention adopts has directly formed microcapsule product, it is to utilize supersonic speed spraying air-flow, make the higher speed difference of gas and liquid (emulsion) two alternate generations, thereby make gas, produce frictional force between the liquid and with the atomization of liquid, the fine droplet of atomizing rotates under the effect of its surface tension and external force and forms hollow ball, in the process that forms hollow ball, polysaccharide gel in the drop forms spherical shell outside, all the other compositions in the drop are wrapped in the ball, thereby form the microcapsules atomized liquid, this microcapsules atomized liquid in spraying into drying tower the time by instantaneous drying.Maximum temperature point control in the tower is below 50 ℃, do not suffer a loss with the physiologically active ingredient of the thing that guarantees to be dried, and the negative pressure in the tower is used to reduce the evaporation point of water droplet, to guarantee instantaneous drying under the low temperature.
In sum, compared with the prior art the present invention has the following advantages:
One, solved the halfway problem of extraction under the low temperature, prepared using is got thoroughly, physiologically active ingredient of plant and specific function composition extract relatively fully, and the repertoire and the whole local flavor that possess plant material for finished product provide necessary condition.Simultaneously, simplify the pulverizing process before the extraction, shortened the extraction time greatly, also avoided the loss of volatile ingredient in crushing process.
Two, solved the moulding problem of microcapsules more satisfactoryly, it can be fully without the wall material, and self form microcapsules with phytochemicals in spray process, and the embedding of this microcapsules, instant capacity and sealing go bad but long preservation is deaden all than using the good of Arabic gum moulding.
Three, solved the dry down problem of low temperature, the physiologically active ingredient of plant is not suffered a loss in drying.
Four, whole technology is carried out under low temperature (being no more than 50 ℃), has guaranteed not suffer a loss in the physiologically active ingredient production of phytochemicals.
The product certification and the accurate font size of new resource food of having obtained Shaanxi Province Department of Public Health { approval number is: No. the 16th, the accurate word in (97) Shan (new food) } of Shaanxi Province Bureau of Technical Supervision have been passed through with the microcapsules xanthoxlin product of the present invention's production.In certificates of recognition, putting down in writing contents such as " are that the Chinese prickly ash monosodium glutamate of raw material production has the spicy strong fragrance of pure natural, fine size, no residue, long shelf-life with Hancheng clovershrub Chinese prickly ash ".Simultaneously, in the company standard of formulating for this product certification, also putting down in writing product requirement and the examination and test of products requirement passed through after evaluation detects in relevant department, taking passages as follows:
One, product requirement
1. organoleptic indicator: should meet table 1 requirement
Table 1
| Project | Index |
| Color and luster, shape | Faint yellow even fine-powdered, free from admixture |
| Flavour, smell | Have whole local flavors of raw material Chinese prickly ash and picotement, free from extraneous odour. |
2. physical and chemical index: should meet table 2 requirement
Table 2
| Project | Index |
| Moisture content (%) | ≤ 5.0 |
| Solubility (%) | 〉=75.0 |
| Discrimination test: | |
| 1. xanthoxylum oleoresin | Positive |
| 2. SEM morphological observation | It is shaped as spheric granules, smooth surface, densification, evenly big or small, and average diameter is about about 50 μ m. |
| Food additives | Meet the GB2760 regulation |
Two, examination and test of products requirement
The 4th of the physical and chemical index check is discrimination test: the sample solution preparation of product; Reference substance solution with the extract before the microencapsulation not (i.e. extraction concentrate and Maillard reaction after oily green pepper fat, volatile essential oil, the mixture of Maillard reaction oil of gained, be referred to as xanthoxylum oleoresin in this standard) preparation, sample solution and reference substance solution are carried out color contrast with ultraviolet and the visible chromatogram method of inspecting, and need to show identical color spot.
From the said goods examination requirements as can be seen: the material behind the packing will with packing before identical, this illustrates that microcapsules moulding process of the present invention can be with the whole embeddings of the phytochemicals that is extracted (comprising difficult formation encapsulated volatile composition).Require " having whole local flavors of raw material Chinese prickly ash and picotement, free from extraneous odour " this Shanghai Stock Exchange the organoleptic indicator to understand that the present invention is more complete to the extraction of Chinese prickly ash phytochemicals from the said goods, simultaneously, confirmed further that also the present invention is with the whole embeddings of Chinese prickly ash phytochemicals of being extracted.From the product form photo of electronic scanner microscope, can be clear that the spherical morphology and the brighter colloid spherical shell of product, thereby understand that from mode of appearance Shanghai Stock Exchange the present invention has formed ball-type capsule by phytochemicals self.In addition, it can also be seen that this product has good solubility and long shelf-life from the physical and chemical index that the said goods requires with in the certificates of recognition, this has proved that product of the present invention has fine instant capacity and seal.
Carry out being applied to the single experiment of meat product with the xanthoxlin of explained hereafter of the present invention, capsicim, allicin, ginger element by " China Meat Comprehensive Study Center ", obtained good effect.In experiment conclusion, putting down in writing characteristics such as " strengthen than fragrance that uses other spice and delicate flavour, delicious flavour have dissolubility, permeability, good dispersion and high-temperature-resistant high-pressure-resistant ".This application experiment has proved that physiological function composition and specific function composition that product of the present invention has a phytochemicals reach the good performance of dissolubility fully, also further confirmed technology of the present invention have extract thoroughly, the desirable advantage of packing.
Describe technical process of the present invention in detail according to embodiment below.
Embodiment 1: the production technology of xanthoxlin
With Shaanxi clovershrub Chinese prickly ash is raw material, removal of impurities; With the 200kg raw material microwave abstracting jar of packing into, the ethanolic solution 380～400kg with 55% carried out microwave abstracting (promptly opening the microwave generator that is contained on the extractor during extracting) 10 minutes, and wherein extraction temperature is 40～45 ℃, extracting pressure 0.12MPA; Then extraction solution is sent in the concentration tank, vacuumized, distillation concentrates under 40～50 ℃ of temperature, gets xanthoxylum oleoresin; Concentrate the steam of discharging and send into rectifying column, separate with proportion, get the ethanolic solution of Chinese prickly ash volatile essential oil and recovery by water circulation cooling; This extraction, concentrated carrying out repeatedly three times; Residue last in the extractor is carried out Maillard reaction, be about to residue and be heated to 110 ℃, be incubated 10 minutes and carry out Maillard reaction, the vapour that evaporates in the reaction is sent into rectifying column, and condensation, separation get Maillard reaction oil; The Chinese prickly ash oil green pepper fat of gained is sent in the mixer, the Tween 80 (emulsifying agent) of adding 0.5%, stir, add 0.5% Arabic gum (antioxidant) again, stir, add volatile essential oil (comprising the Maillard reaction oil that combines) and following auxiliary material more successively: 0.1% calcium phosphate (anticaking agent), 2.5% carboxymethyl are tieed up plain sodium (anti-blushing agent), 10% maltodextrin (filler), 5% β dextrin (antioxidant), stir; Send in the homogenizer homogeneous under 25MPa pressure again; Then the emulsion behind the homogeneous is pumped in the supersonic speed spraying negative pressure drying tower and carry out spray-drying, get microcapsules xanthoxlin product, wherein pump pressure is 0.6MPa, the spraying flow velocity is 800 meter per seconds, the temperature in maximum temperature distributed area is 40～50 ℃ in the tower, EAT is 80～120 ℃, and leaving air temp is 25～35 ℃, and negative pressure is 0.02～0.03MPa in the tower.The maximum temperature distributed area is provided with a temperature sensor (as: thermocouple) in the tower, surveys this regional temperature with it, and the hot blast rate in the tower is sent in control then, is no more than 50 ℃ to guarantee this regional temperature.Negative pressure realizes by vacuumizing in the tower.
Embodiment 2: the production technology of allicin
With the 200kg garlic extractor of packing into, the ethanolic solution 400～420kg with 60% press embodiment 1 the method extraction, concentrate three times, garlic oleoresin and volatile essential oil, wherein extraction temperature is 35～40 ℃, extracting pressure is 0.08～0.1Mpa; Extraction residue is heated to 110～120 ℃ carries out Maillard reaction, get reaction oil; The Tween 80 of adding 0.1% stirs in garlic oleoresin; Add volatile essential oil again, stir; Homogeneous; Supersonic speed spraying negative pressure drying gets white fine powder shape microcapsule product then, and wherein the interior temperature of tower is 40～45 ℃, and EAT is 80～90 ℃, 25～32 ℃ of leaving air temps.
Embodiment 3: the production technology of gynostemma pentaphylla element
With the 200kg gynostemma pentaphylla raw material extractor of packing into, the ethanolic solution 420～440kg with 55% press embodiment 1 the method extraction, concentrate secondary, gynostemma pentaphylla oleoresin and volatile essential oil, 35～40 ℃ of extraction temperature, pressure is 0.08Mpa; With extraction residue heating carrying out Maillard reaction, get reaction oil; The Tween 80 of adding 0.1% stirs in oleoresin; Add volatile essential oil again, stir; Homogeneous; Supersonic speed spraying negative pressure drying then, particle diameter is a coffee-like microcapsule product about 10 μ m, drying condition is same with embodiment 1.
Embodiment 4: the production technology of angelicin
With the 200kg Radix Angelicae Sinensis raw material extractor of packing into, the ethanolic solution 380～400kg with 55% press embodiment 1 the method extraction, concentrate three times, Radix Angelicae Sinensis oleoresin and volatile essential oil, 40～45 ℃ of extraction temperature, pressure is 0.1Mpa; With extraction residue heating carrying out Maillard reaction, get reaction oil; The Tween 80 of adding 0.2% stirs in oleoresin; Add ethereal oil again, stir; Homogeneous; Supersonic speed spraying negative pressure drying then, particle diameter is a dark brown microcapsule product about 10 μ m, drying condition is same with embodiment 1.
Embodiment 5, the production technology of instant tea
With the 200kg tealeaves extractor of packing into, with the about 450kg of 70% ethanolic solution press embodiment 1 the method extraction, concentrate secondary, tea extract and volatile essential oil, wherein extraction temperature is 40～45 ℃, pressure 0.06～0.08MPa; Extraction residue is heated to 110～120 ℃ carries out Maillard reaction, get reaction oil; Tea extract and volatile essential oil are mixed, stir; Homogeneous under 15～20Mpa; Supersonic speed spraying negative pressure drying then, particle diameter is a coffee-like microcapsule product about 10 μ m, drying condition is same with embodiment 1.
Embodiment 6, the production technology of peanut grease and defatted peanut rice
With the 200kg shelled peanut extractor of packing into, with the about 500kg of 90% ethanolic solution press embodiment 1 the method extraction, concentrate three times, peanut extract and peanut essential oil, wherein extraction temperature is 40～45 ℃, pressure 0.06～0.08MPa; Shelled peanut after extracting in oven dry below 50 ℃, is got defatted peanut rice; Peanut extract and peanut oil are mixed, stir; Homogeneous; Supersonic speed spraying negative pressure drying gets faint yellow microcapsules peanut oil fat prod then, and drying condition and embodiment 1 are together.
By the foregoing description 3～6 as can be seen, doping hardly in the technology, thus guaranteed the purity of Chinese herbal medicine product and the natural sex of food product.
Claims (2)
1, a kind of production method of microcapsule plant extract is characterized in that its method step is as follows:
1.1, the extraction of plant oil resin: plant material is put into the microwave abstracting jar carries out the microwave solvent extraction, 35～45 ℃ of extraction temperature, pressure 0.06～0.12Mpa, solution after the extraction is sent into concentration tank, vacuumize distillation and concentrate, get plant oil resin or plant extracts, thickening temperature is lower than 50 ℃, vaporized gas is sent into rectifying column in concentrating, and obtains phytovolatilization essential oil and recovered solvent by condensation, separation;
1.2, Maillard reaction: will extract 100～120 ℃ of last plant residue heating, be incubated 10～20 minutes, making plant residue is that catalyst at high temperature produces Maillard reaction with residual solvent, the plant heteroaromatic composition that evaporates in the reaction enters rectifying column, obtains Maillard reaction oil by condensation, separation;
1.3, the emulsification of plant oil resin and emulsion or plant extracts mix with Maillard reaction oil and volatile essential oil: the standard adding emulsifying agent of press the state food additive in the plant oil resin of extraction gained, stir, add the Maillard reaction oil and the phytovolatilization essential oil of gained again, stir; Perhaps will extract plant extracts and the phytovolatilization essential oil and the directly mixing of Maillard reaction oil of gained, stir;
1.4, homogeneous: the emulsion that mixes or extract mixing liquid are sent in the homogenizer homogeneous under 15～25Mpa, obtain emulsion;
1.5, supersonic speed spraying negative pressure drying: the emulsion of homogeneous gained sent in the supersonic speed spraying negative pressure drying machine is dried to the plant microcapsule product, the flow velocity of supersonic speed spraying is 340～800 meter per seconds under pressure 0.4～0.7Mpa, the tower inner drying is to limit maximum temperature in the tower, to limit EAT and leaving air temp is auxilliary, be that the highest temperature zone temperature is defined as 40～50 ℃ in the tower, and the negative pressure with 0.02～0.03Mpa is moved in the tower.
2, the production method of microcapsule plant extract as claimed in claim 1 is characterized in that: the flow velocity of described supersonic speed spraying is to be 800 meter per seconds under 0.4～0.7Mpa at pressure.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB991159047A CN1163155C (en) | 1999-11-10 | 1999-11-10 | Productive technology for microcapsule plant extract |
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| Application Number | Priority Date | Filing Date | Title |
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| CNB991159047A CN1163155C (en) | 1999-11-10 | 1999-11-10 | Productive technology for microcapsule plant extract |
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| CN1295805A CN1295805A (en) | 2001-05-23 |
| CN1163155C true CN1163155C (en) | 2004-08-25 |
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| CNB991159047A Expired - Fee Related CN1163155C (en) | 1999-11-10 | 1999-11-10 | Productive technology for microcapsule plant extract |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100462121C (en) * | 2006-10-23 | 2009-02-18 | 天水华圆制药设备科技有限责任公司 | Continuous extracting method of microwave |
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| CN100367944C (en) * | 2004-11-19 | 2008-02-13 | 中国海洋大学 | Allicin microcapsule and its preparation method |
| CN101278897B (en) * | 2008-04-25 | 2010-06-09 | 西安交通大学 | Process for preparing brevifolin solid lipid nano particle |
| CN101755955B (en) * | 2009-09-29 | 2013-04-10 | 刘宝 | Solid-state instant tea granule and preparation method thereof |
| CN103229857A (en) * | 2013-04-25 | 2013-08-07 | 西华大学 | Quenching and extracting process of onion oil and garlic oil |
| US10202497B2 (en) | 2015-09-10 | 2019-02-12 | Bridgestone Corporation | Microwave extraction technique for rubber and resin analysis |
| CN108244455A (en) * | 2017-12-19 | 2018-07-06 | 安徽强旺生物工程有限公司 | A kind of high efficiency extraction technique of natural flavor |
| CN108651709A (en) * | 2018-03-26 | 2018-10-16 | 味氏（广东）生物科技股份有限公司 | Antibacterial bacteriostatic growth accelerator and its preparation method and application |
| CN108967987A (en) * | 2018-06-20 | 2018-12-11 | 漯河双汇生物工程技术有限公司 | A kind of garlicky essence of blending type and preparation method thereof |
| CN113907316A (en) * | 2021-10-27 | 2022-01-11 | 福建正味生物科技有限公司 | Plant modifier and preparation method thereof |
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1999
- 1999-11-10 CN CNB991159047A patent/CN1163155C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100462121C (en) * | 2006-10-23 | 2009-02-18 | 天水华圆制药设备科技有限责任公司 | Continuous extracting method of microwave |
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