MD557Z - Process for microencapsulation of food and cosmetic oil compositions - Google Patents
Process for microencapsulation of food and cosmetic oil compositions Download PDFInfo
- Publication number
- MD557Z MD557Z MDS20120073A MDS20120073A MD557Z MD 557 Z MD557 Z MD 557Z MD S20120073 A MDS20120073 A MD S20120073A MD S20120073 A MDS20120073 A MD S20120073A MD 557 Z MD557 Z MD 557Z
- Authority
- MD
- Moldova
- Prior art keywords
- oil
- extract
- microencapsulation
- food
- temperature
- Prior art date
Links
- 238000000034 method Methods 0.000 title claims abstract description 20
- 235000013305 food Nutrition 0.000 title claims abstract description 18
- 239000002537 cosmetic Substances 0.000 title claims abstract description 17
- 239000000203 mixture Substances 0.000 title claims abstract description 15
- 239000003094 microcapsule Substances 0.000 claims abstract description 36
- 108010010803 Gelatin Proteins 0.000 claims abstract description 35
- 239000008273 gelatin Substances 0.000 claims abstract description 35
- 229920000159 gelatin Polymers 0.000 claims abstract description 35
- 235000019322 gelatine Nutrition 0.000 claims abstract description 35
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 35
- 239000000284 extract Substances 0.000 claims abstract description 32
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims abstract description 24
- 229910052938 sodium sulfate Inorganic materials 0.000 claims abstract description 24
- 235000011152 sodium sulphate Nutrition 0.000 claims abstract description 24
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000000126 substance Substances 0.000 claims abstract description 11
- 241001122767 Theaceae Species 0.000 claims abstract description 7
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000000926 separation method Methods 0.000 claims abstract description 4
- 239000006286 aqueous extract Substances 0.000 claims abstract 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 241001474374 Blennius Species 0.000 claims description 11
- 239000010495 camellia oil Substances 0.000 claims description 10
- 239000003921 oil Substances 0.000 claims description 8
- 230000001804 emulsifying effect Effects 0.000 claims description 3
- 239000012528 membrane Substances 0.000 abstract description 15
- 241000195493 Cryptophyta Species 0.000 abstract description 11
- 108090000623 proteins and genes Proteins 0.000 abstract description 3
- 102000004169 proteins and genes Human genes 0.000 abstract description 3
- 239000013543 active substance Substances 0.000 abstract description 2
- 238000004945 emulsification Methods 0.000 abstract description 2
- 238000010525 oxidative degradation reaction Methods 0.000 abstract description 2
- 238000002360 preparation method Methods 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 37
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 21
- 239000000839 emulsion Substances 0.000 description 18
- 230000015572 biosynthetic process Effects 0.000 description 8
- 235000019198 oils Nutrition 0.000 description 7
- 239000007832 Na2SO4 Substances 0.000 description 6
- 238000010908 decantation Methods 0.000 description 6
- 239000007864 aqueous solution Substances 0.000 description 5
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 4
- 235000019486 Sunflower oil Nutrition 0.000 description 4
- 238000002156 mixing Methods 0.000 description 4
- 239000002600 sunflower oil Substances 0.000 description 4
- 235000021466 carotenoid Nutrition 0.000 description 3
- 150000001747 carotenoids Chemical class 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 3
- 238000005345 coagulation Methods 0.000 description 3
- 230000015271 coagulation Effects 0.000 description 3
- 239000012141 concentrate Substances 0.000 description 3
- 230000003247 decreasing effect Effects 0.000 description 3
- 229920000609 methyl cellulose Polymers 0.000 description 3
- 239000001923 methylcellulose Substances 0.000 description 3
- 239000000654 additive Substances 0.000 description 2
- 235000019658 bitter taste Nutrition 0.000 description 2
- 238000009833 condensation Methods 0.000 description 2
- 230000005494 condensation Effects 0.000 description 2
- 230000005294 ferromagnetic effect Effects 0.000 description 2
- 239000000499 gel Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000010583 slow cooling Methods 0.000 description 2
- 230000006641 stabilisation Effects 0.000 description 2
- 238000011105 stabilization Methods 0.000 description 2
- 230000000087 stabilizing effect Effects 0.000 description 2
- 235000019640 taste Nutrition 0.000 description 2
- 239000007900 aqueous suspension Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005538 encapsulation Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 239000008169 grapeseed oil Substances 0.000 description 1
- 239000002609 medium Substances 0.000 description 1
- 230000020477 pH reduction Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920005597 polymer membrane Polymers 0.000 description 1
- 230000002028 premature Effects 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 235000020183 skimmed milk Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 230000009967 tasteless effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000003809 water extraction Methods 0.000 description 1
Landscapes
- Cosmetics (AREA)
- Fats And Perfumes (AREA)
Abstract
Description
Invenţia se referă la industria alimentară şi cosmetică, şi anume la un procedeu de microîncapsulare a compoziţiilor alimentare şi cosmetice uleioase, în scopul protejării de degradări oxidative şi menţinerii în stare naturală a substanţelor biologic active liposolubile. The invention relates to the food and cosmetic industry, namely to a process for microencapsulating oily food and cosmetic compositions, in order to protect them from oxidative degradation and maintain the natural state of liposoluble biologically active substances.
Este cunoscut un procedeu de obţinere a microcapsulelor, care include emulsionarea materialului de microîncapsulare în soluţie de gelatină în prezenţa aditivilor, care micşorează solubilitatea gelatinei în soluţii apoase, favorizează condensarea gelatinei pe suprafaţa picăturilor emulsiei cu formarea ulterioară a membranelor polimerice în stare solidă. În calitate de aditivi se utilizează particule feromagnetice, iar pentru formarea şi fortificarea membranelor se utilizează soluţii ale sărurilor metalelor polivalente [1]. A process for obtaining microcapsules is known, which includes emulsifying the microencapsulating material in gelatin solution in the presence of additives, which reduce the solubility of gelatin in aqueous solutions, favor the condensation of gelatin on the surface of the emulsion droplets with the subsequent formation of solid-state polymer membranes. Ferromagnetic particles are used as additives, and solutions of polyvalent metal salts are used for the formation and strengthening of membranes [1].
Dezavantajul procedeului cunoscut constă în necesitatea adăugării substanţelor feromagnetice şi a unor cantităţi esenţiale de săruri ale metalelor polivalente, ceea ce nu este binevenit pentru utilizarea ulterioară a microcapsulelor în industria alimentară şi cosmetică. The disadvantage of the known process consists in the need to add ferromagnetic substances and essential quantities of polyvalent metal salts, which is not welcome for the subsequent use of microcapsules in the food and cosmetic industry.
Mai este cunoscut un procedeu de microîncapsulare a substanţelor cu gust şi aromă pentru obţinerea produselor alimentare fără gust şi aromă, care include utilizarea laptelui-praf degresat în calitate de agent de microîncapsulare, introducerea dozată a substanţelor cu gust şi aromă cu ajutorul unei micropompe, uscarea ulterioară a emulsiei omogenizate prin dispersare cu obţinerea unui produs în stare de pulbere [2]. There is also a known process for microencapsulating taste and aroma substances to obtain tasteless and aromaless food products, which includes the use of skimmed milk powder as a microencapsulating agent, the dosed introduction of taste and aroma substances using a micropump, and the subsequent drying of the homogenized emulsion by dispersion to obtain a powder product [2].
Dezavantajele procedeului cunoscut constau în cantitatea mică de substanţe în componenţa microcapsulelor şi stabilitatea scăzută a lor, care se manifestă prin păstrarea aromei substanţelor microîncapsulate în produsul finit, ceea ce confirmă faptul difuziei substanţei microîncapsulate prin membranele microcapsulelor. The disadvantages of the known process consist in the small amount of substances in the composition of the microcapsules and their low stability, which is manifested by the preservation of the aroma of the microencapsulated substances in the finished product, which confirms the diffusion of the microencapsulated substance through the membranes of the microcapsules.
Cea mai apropiată soluţie de procedeul propus include emulsionarea substanţei încapsulate în soluţie de metilceluloză, formarea membranelor microcapsulelor prin condensarea metilcelulozei pe suprafaţa picăturilor emulsiei, înlăturarea excesului fazei uleioase prin intermediul acetonei. Ca rezultat se obţine suspensia apoasă a microcapsulelor [3]. The closest solution to the proposed process includes emulsifying the encapsulated substance in methylcellulose solution, forming microcapsule membranes by condensation of methylcellulose on the surface of the emulsion droplets, removing the excess oil phase by acetone. As a result, an aqueous suspension of microcapsules is obtained [3].
Printre dezavantajele acestui procedeu poate fi menţionată utilizarea în calitate de material pentru obţinerea membranelor a metilcelulozei şi prelucrarea microcapsulelor cu acetonă, care este toxică şi inflamabilă. Among the disadvantages of this process can be mentioned the use of methylcellulose as a material for obtaining membranes and the processing of microcapsules with acetone, which is toxic and flammable.
Problema, pe care o rezolvă invenţia propusă, este elaborarea unui procedeu de microîncapsulare a compoziţiilor alimentare şi cosmetice liposolubile, care exclude pierderea fazei uleioase biologic active, iar microcapsulele obţinute conţin doar substanţe acceptabile în industria alimentară şi cosmetică. The problem, which the proposed invention solves, is the development of a microencapsulation process for liposoluble food and cosmetic compositions, which excludes the loss of the biologically active oily phase, and the obtained microcapsules contain only substances acceptable in the food and cosmetic industry.
Procedeul de microîncapsulare a compoziţiilor alimentare şi cosmetice uleioase include prepararea compoziţiei alimentare şi cosmetice uleioase ce conţine substanţe liposolubile şi 1,0...10,0% de extract uleios de ceai, emulsionarea acesteia în soluţie apoasă de gelatină de 3,0...4,0% cu pH-ul de 2,5...5,0 la agitare cu viteza de 300...450 rot/min la temperatura de 75...90°C, micşorarea temperaturii până la 15...20°C şi a vitezei de agitare până la 25...75 rot/min, tratarea cu soluţie de sulfat de sodiu de 12...16% în raport de 1:1, spălarea dublă a microcapsulelor formate cu extract apos de alge marine şi separarea lor ulterioară. The microencapsulation process of oily food and cosmetic compositions includes the preparation of the oily food and cosmetic composition containing liposoluble substances and 1.0...10.0% of tea oil extract, its emulsification in an aqueous gelatin solution of 3.0...4.0% with a pH of 2.5...5.0 while stirring at a speed of 300...450 rpm at a temperature of 75...90°C, lowering the temperature to 15...20°C and the stirring speed to 25...75 rpm, treatment with a 12...16% sodium sulfate solution in a 1:1 ratio, double washing of the formed microcapsules with aqueous seaweed extract and their subsequent separation.
Procedeul de microîncapsulare a compoziţiilor alimentare şi cosmetice uleioase constă în prepararea fazei uleioase pentru microîncapsulare, care conţine extract uleios de ceai, extracţia algelor marine, prepararea soluţiilor de gelatină şi de sulfat de sodiu, modelarea pH-ului soluţiei de gelatină cu acid citric, obţinerea şi stabilizarea emulsiei ulei/apă (U/A), formarea membranelor microcapsulelor prin tratarea cu soluţie de sulfat de sodiu, desulfatarea şi stabilizarea microcapsulelor cu extract de alge marine, urmată de decantarea sau centrifugarea lor, în care faza uleioasă supusă microîncapsulării conţine 1,0...10% de extract uleios de ceai; pH-ul soluţiei apoase de gelatină se modelează cu acid citric în intervalul 2,5...5,0; emulsia ulei/apă se formează prin agitarea fazei uleioase şi a soluţiei de gelatină la temperatura de 75...90°C cu viteza de 300...450 rot/min; emulsia se stabilizează prin răcirea lentă până la 15...20°C şi prin micşorarea vitezei de agitare până la 25...75 rot/min; formarea membranelor microcapsulelor are loc prin adăugarea soluţiei de sulfat de sodiu de 12...16% în raport de 1:1; desulfitarea şi stabilizarea microcapsulelor are loc prin tratarea acestora în două etape cu extract de alge 10% (1/4 din volumul total), iar separarea microcapsulelor are loc prin decantare sau centrifugare. The microencapsulation process of oily food and cosmetic compositions consists of preparing the oily phase for microencapsulation, which contains tea oil extract, seaweed extraction, preparing gelatin and sodium sulfate solutions, modeling the pH of the gelatin solution with citric acid, obtaining and stabilizing the oil/water emulsion (U/A), forming the microcapsule membranes by treating with sodium sulfate solution, desulfating and stabilizing the microcapsules with seaweed extract, followed by their decantation or centrifugation, in which the oily phase subjected to microencapsulation contains 1.0...10% of tea oil extract; the pH of the aqueous gelatin solution is modeled with citric acid in the range of 2.5...5.0; the oil/water emulsion is formed by stirring the oily phase and the gelatin solution at a temperature of 75...90°C with a speed of 300...450 rpm; the emulsion is stabilized by slow cooling to 15...20°C and by decreasing the stirring speed to 25...75 rpm; the formation of microcapsule membranes occurs by adding 12...16% sodium sulfate solution in a 1:1 ratio; desulfitization and stabilization of microcapsules occurs by treating them in two stages with 10% algae extract (1/4 of the total volume), and the separation of microcapsules occurs by decantation or centrifugation.
Rezultatul constă în microîncapsularea completă a fazei uleioase şi obţinerea microcapsulelor cu membrană proteică comestibilă, stabile mecanic, termic şi chimic. The result is the complete microencapsulation of the oily phase and the obtaining of edible protein membrane microcapsules, mechanically, thermally and chemically stable.
Rezultatul se datorează faptului că faza uleioasă, supusă microîncapsulării, conţine 1,0-10,0% de extract uleios de ceai, care iniţiază procesul de formare a membranelor proteice; concentraţia soluţiilor de gelatină este de 3,0...4,0%, iar pH-ul lor se modelează cu acid citric în limitele 2,5...5,0, în care microcapsulele au stabilitate mecanică înaltă; emulsia U/A se formează prin agitarea compoziţiei alimentare sau cosmetice uleioase supusă microîncapsulării şi a soluţiei de gelatină la temperatura de 75...90°C cu viteza de 300...450 rot/min, ce asigură mărimea necesară şi stabilitatea mecanică ulterioară a microcapsulelor; emulsia se stabilizează prin răcirea lentă până la 15...20°C şi micşorarea lentă a vitezei de agitare până la 25...75 rot/min, ce asigură stabilitatea fazelor emulsiei şi formarea membranelor microcapsulelor; membranele microcapsulelor se deshidratează prin adăugarea soluţiei de sulfat de sodiu de 12...16% în raport de 1:1, pentru a asigura formarea membranelor şi a evita coagularea prematură a gelatinei; microcapsulele se desulfatează şi se stabilizează prin spălarea dublă cu extractul de alge marine de 10% (1/4 din volumul total), astfel îşi pierd gustul amar, caracteristic sulfatului de sodiu. The result is due to the fact that the oily phase, subjected to microencapsulation, contains 1.0-10.0% of tea oil extract, which initiates the process of protein membrane formation; the concentration of gelatin solutions is 3.0...4.0%, and their pH is modeled with citric acid within the limits of 2.5...5.0, in which the microcapsules have high mechanical stability; the U/A emulsion is formed by stirring the oily food or cosmetic composition subjected to microencapsulation and the gelatin solution at a temperature of 75...90°C with a speed of 300...450 rpm, which ensures the necessary size and subsequent mechanical stability of the microcapsules; the emulsion is stabilized by slow cooling to 15...20°C and slow reduction of the stirring speed to 25...75 rpm, which ensures the stability of the emulsion phases and the formation of the microcapsule membranes; the microcapsule membranes are dehydrated by adding 12...16% sodium sulfate solution in a 1:1 ratio, to ensure membrane formation and avoid premature gelatin coagulation; the microcapsules are desulfated and stabilized by double washing with 10% seaweed extract (1/4 of the total volume), thus losing their bitter taste, characteristic of sodium sulfate.
Faza uleioasă în care extractul uleios de ceai depăşeşte limitele 1,0...10,0% nu se microîncapsulează complet. Concentraţiile de gelatină mai mici de 3,0% nu asigură încapsularea completă, iar la concentraţii de gelatină mai mari de 4,0% suspensia se gelifică. La pH < 2,5 a soluţiei de gelatină membranele microcapsulelor îşi pierd elasticitatea şi se sparg foarte uşor la acţiune mecanică, iar la pH > 5 devin moi şi amorfe, ceea ce duce la microîncapsularea incompletă a uleiului. Formarea emulsiei U/A la temperaturi mai mici de 75°C şi la viteza < 300 rot/min duce la mărirea dimensiunilor picăturilor de ulei, la temperaturi mai mari de 90°C este posibilă degradarea compoziţiei alimentare sau cosmetice uleioase supusă microîncapsulării, la viteza > 450 rot/min se formează o spumă stabilă, care împiedică microîncapsularea ulterioară. Scăderea rapidă a vitezei de agitare şi răcirea bruscă duc la gelificarea emulsiei, împiedecând procesul de formare a membranelor microcapsulelor. Adăugarea soluţiei de sulfat de sodiu cu concentraţia < 12% nu asigură stabilizarea membranelor gelatinoase, iar la concentraţia soluţiei de sulfat de sodiu > 16% se formează un sediment mărunt nedorit în timpul administrării soluţiei în reactor, provocând coagularea gelatinei. O singură spălare a microcapsulelor cu extractul de alge marine de 10% (1/4 din volum total) nu asigură desulfatarea lui completă. The oily phase in which the tea oil extract exceeds the limits of 1.0...10.0% is not completely microencapsulated. Gelatin concentrations lower than 3.0% do not ensure complete encapsulation, and at gelatin concentrations higher than 4.0% the suspension gels. At pH < 2.5 of the gelatin solution, the microcapsule membranes lose their elasticity and break very easily under mechanical action, and at pH > 5 they become soft and amorphous, which leads to incomplete microencapsulation of the oil. The formation of the U/A emulsion at temperatures lower than 75°C and at speeds < 300 rpm leads to an increase in the size of the oil droplets, at temperatures higher than 90°C, degradation of the oily food or cosmetic composition subjected to microencapsulation is possible, at speeds > 450 rpm a stable foam is formed, which prevents further microencapsulation. The rapid decrease in the stirring speed and sudden cooling lead to gelation of the emulsion, preventing the process of forming microcapsule membranes. The addition of sodium sulfate solution with a concentration of < 12% does not ensure the stabilization of gelatinous membranes, and at a sodium sulfate solution concentration of > 16%, an undesirable fine sediment is formed during the administration of the solution into the reactor, causing gelatin coagulation. A single washing of the microcapsules with 10% seaweed extract (1/4 of the total volume) does not ensure its complete desulfation.
Argumentarea necesităţii respectării condiţiilor optime, indicate pentru realizarea procedeului de microîncapsulare a compoziţiilor alimentare şi cosmetice uleioase, se ilustrează prin exemple concrete de realizare, unii parametri fiind menţionaţi în tabel. The argumentation of the need to respect the optimal conditions, indicated for carrying out the microencapsulation process of oily food and cosmetic compositions, is illustrated by concrete examples of implementation, some parameters being mentioned in the table.
Exemple de realizare a procedeului Examples of process implementation
Exemplul 1 Example 1
Se pregăteşte mai întâi extractul de alge prin extracţia cu apă a algelor uscate (raportul alge : apă de 1 : 9) la 80°C, 1...2 ore, după care reziduul solid se centrifughează, apoi soluţiile apoase de gelatină (2 g gelatină, 98 ml apă) şi de sulfat de sodiu (20 g Na2SO4, 80 ml apă). Soluţia de gelatină se aduce la pH = 5,5 prin acidulare cu acid citric. Faza uleioasă, supusă microîncapsulării, se pregăteşte prin amestecarea a 9 ml de ulei de floarea-soarelui cu 3,0 ml de concentrat de carotinoide. Soluţia de gelatină se agită la temperatura camerei cu viteza de 100 rot/min. În această soluţie se adaugă rapid faza uleioasă. Emulsia obţinută se amestecă continuu la aceeaşi viteză şi temperatură timp de 2 ore. În emulsie se administrează soluţia de sulfat de sodiu cu viteza de debitare de 4,0 ml/min. Pe lângă microcapsulele ca atare în soluţie se formează cheaguri de microcapsule. Acestea se înlătură mecanic, apoi în reactor se adaugă 50 ml de extract de alge. Agitarea continuă încă 40 min. La oprirea agitatorului microcapsulele formează un strat superior afânat, care mai conţine cca 5...10% de fază uleioasă în stare liberă (neîncapsulată). Produsul se separă prin multiple decantări. First, the algae extract is prepared by water extraction of dried algae (algae:water ratio 1:9) at 80°C, 1...2 hours, after which the solid residue is centrifuged, then the aqueous solutions of gelatin (2 g gelatin, 98 ml water) and sodium sulfate (20 g Na2SO4, 80 ml water). The gelatin solution is brought to pH = 5.5 by acidification with citric acid. The oily phase, subjected to microencapsulation, is prepared by mixing 9 ml of sunflower oil with 3.0 ml of carotenoid concentrate. The gelatin solution is stirred at room temperature at a speed of 100 rpm. The oily phase is quickly added to this solution. The emulsion obtained is continuously stirred at the same speed and temperature for 2 hours. The sodium sulfate solution is fed into the emulsion at a flow rate of 4.0 ml/min. In addition to the microcapsules themselves, microcapsule clots form in the solution. These are removed mechanically, then 50 ml of algae extract is added to the reactor. Stirring is continued for another 40 min. When the stirrer is turned off, the microcapsules form a loose upper layer, which still contains about 5...10% of the free (unencapsulated) oily phase. The product is separated by multiple decantations.
Exemplul 2 Example 2
Se pregăteşte extractul de alge marine conform Exemplului 1. Se pregăteşte extractul uleios de ceai prin extracţia cu ulei de floarea-soarelui a frunzelor uscate de ceai în raport de 5 : 1, la 80…90°C, timp de 1…2 ore, apoi urmează filtrarea extractului. Se pregătesc soluţiile apoase de gelatină (3,0 g gelatină, 97 ml apă) şi de sulfat de sodiu (10 g Na2SO4, 90 ml apă). pH-ul soluţiei de gelatină se aduce la 2,0 prin adăugarea acidului citric. Faza uleioasă, supusă microîncapsulării, se pregăteşte prin amestecarea a 9,9 ml de ulei din seminţe de struguri cu 0,1 ml de extract de ceai. Soluţia de gelatină la temperatura de 95°C se agită la 200 rot/min. În această soluţie se adaugă rapid faza uleioasă. Fazele se amestecă continuu, la viteză constantă şi temperatură scadentă, timp de 1 oră. În emulsia obţinută se administrează soluţia de sulfat de sodiu cu viteza de debitare de 10 ml/min. Pe lângă microcapsule, în soluţie mai rămân cca 2% de ulei în stare liberă (neîncapsulat). Agitarea continuă încă 40 min. La oprirea agitatorului microcapsulele formează un strat superior afânat, iar mediul de dispersie, în care se află acestea, se gelifică. În amestecul obţinut se adaugă 50 ml de extract de alge, iar peste 30 min microcapsulele se decantează. Prepare the seaweed extract according to Example 1. Prepare the tea oil extract by extracting the dried tea leaves with sunflower oil in a ratio of 5:1, at 80…90°C, for 1…2 hours, then filter the extract. Prepare the aqueous solutions of gelatin (3.0 g gelatin, 97 ml water) and sodium sulfate (10 g Na2SO4, 90 ml water). The pH of the gelatin solution is brought to 2.0 by adding citric acid. The oily phase, subjected to microencapsulation, is prepared by mixing 9.9 ml of grape seed oil with 0.1 ml of tea extract. The gelatin solution at a temperature of 95°C is stirred at 200 rpm. The oily phase is quickly added to this solution. The phases are continuously mixed, at a constant speed and low temperature, for 1 hour. The sodium sulfate solution is added to the obtained emulsion at a flow rate of 10 ml/min. In addition to the microcapsules, about 2% of free oil (unencapsulated) remains in the solution. Stirring is continued for another 40 min. When the stirrer is stopped, the microcapsules form a loose upper layer, and the dispersion medium in which they are located gels. 50 ml of algae extract is added to the obtained mixture, and after 30 min the microcapsules are decanted.
Exemplul 3 Example 3
Se pregăteşte extractul de alge marine conform Exemplului 1, iar extractul uleios de ceai conform Exemplului 2. Se pregătesc soluţiile apoase de gelatină (3,0 g gelatină, 97 ml apă) şi de sulfat de sodiu (12 g Na2SO4, 88 ml apă). Soluţia de gelatină se aduce la pH = 5,0 cu acid citric. Faza uleioasă, supusă microîncapsulării, se pregăteşte prin amestecarea a 8 ml de ulei de floarea-soarelui, 2,8 ml de concentrat de carotinoide, 1,2 ml de extract de ceai. Soluţia de gelatină se aduce la 75°C şi viteza de agitare de 300 rot/min. În această soluţie se adaugă cu picătura faza uleioasă, adusă la 75°C. Fazele se amestecă continuu, scăzând viteza de agitare concomitent cu scăderea temperaturii până la temperatura de 25°C şi viteza de 75 rot/min. Apoi viteza de agitare şi temperatura emulsiei se menţin constante. În emulsie se administrează soluţia de sulfat de sodiu cu viteza de debitare de 2 ml/min. Apoi în reactor se adaugă 50 ml de extract de alge, agitarea continuă încă cca 40 min. La oprirea agitatorului microcapsulele formează un strat superior compact, care se separă prin decantare. Microcapsulele se mai spală cu încă 50 ml de extract de alge, apoi se separă prin decantare. Prepare the seaweed extract according to Example 1, and the tea oil extract according to Example 2. Prepare the aqueous solutions of gelatin (3.0 g gelatin, 97 ml water) and sodium sulfate (12 g Na2SO4, 88 ml water). The gelatin solution is brought to pH = 5.0 with citric acid. The oily phase, subjected to microencapsulation, is prepared by mixing 8 ml of sunflower oil, 2.8 ml of carotenoid concentrate, 1.2 ml of tea extract. The gelatin solution is brought to 75°C and the stirring speed is 300 rpm. The oily phase, brought to 75°C, is added dropwise to this solution. The phases are continuously mixed, decreasing the stirring speed simultaneously with the temperature decrease to 25°C and the speed of 75 rpm. Then the stirring speed and the temperature of the emulsion are kept constant. The sodium sulfate solution is fed into the emulsion at a flow rate of 2 ml/min. Then 50 ml of algae extract are added to the reactor, stirring is continued for another 40 min. When the stirrer is stopped, the microcapsules form a compact upper layer, which is separated by decantation. The microcapsules are washed with another 50 ml of algae extract, then separated by decantation.
Exemplul 4 Example 4
Se pregăteşte extractul de alge marine conform Exemplului 1, iar extractul uleios de ceai conform Exemplului 2. Se pregătesc soluţiile apoase de gelatină (4,0 g gelatină, 96 ml apă) şi de sulfat de sodiu (16 g Na2SO4, 84 ml apă). Soluţia de gelatină se aduce la pH = 2,5 prin adăugarea acidului citric. Faza uleioasă, supusă microîncapsulării, se pregăteşte prin amestecarea a 7 ml ulei de floarea-soarelui, 4,4 ml de concentrat de carotinoide şi 0,6 ml de extract de ceai. Soluţia de gelatină se aduce la 90°C şi viteza de agitare de 450 rot/min. În această soluţie se adaugă rapid faza uleioasă, adusă la 90°C. Fazele se amestecă continuu, scăzând concomitent viteza de agitare şi temperatura până la 25 rot/min şi 15°C. Apoi viteza de agitare şi temperatura emulsiei se menţin constante. În emulsia obţinută se administrează soluţia de sulfat de sodiu cu viteza de debitare de 2,5 ml/min. În sistemul format se adaugă 50 ml de extract de alge; agitarea continuă încă cca 40 min. La deconectarea agitatorului microcapsulele formează un strat superior compact, care se separă uşor prin decantare. Microcapsulele se mai spală o dată cu 50 ml de extract de alge, apoi se separă prin centrifugare. Prepare the seaweed extract according to Example 1, and the tea oil extract according to Example 2. Prepare the aqueous solutions of gelatin (4.0 g gelatin, 96 ml water) and sodium sulfate (16 g Na2SO4, 84 ml water). The gelatin solution is brought to pH = 2.5 by adding citric acid. The oily phase, subjected to microencapsulation, is prepared by mixing 7 ml sunflower oil, 4.4 ml carotenoid concentrate and 0.6 ml tea extract. The gelatin solution is brought to 90°C and the stirring speed is 450 rpm. The oily phase, brought to 90°C, is quickly added to this solution. The phases are continuously mixed, simultaneously decreasing the stirring speed and temperature to 25 rpm and 15°C. Then the stirring speed and the temperature of the emulsion are kept constant. The sodium sulfate solution is added to the obtained emulsion at a flow rate of 2.5 ml/min. 50 ml of algae extract are added to the formed system; stirring is continued for about 40 min. When the stirrer is disconnected, the microcapsules form a compact upper layer, which is easily separated by decantation. The microcapsules are washed once more with 50 ml of algae extract, then separated by centrifugation.
Compararea eficienţei exemplelor, referitoare la realizarea invenţiei. Comparison of the effectiveness of the examples, relating to the implementation of the invention.
Tabel Table
№ Extract uleios de ceai Gelatină, % Gelatină, pH Na2SO4 Prezenţa de ulei neîncapsulat Formarea sedimentului de Na2SO4 Coagularea produsului Stabilitatea mecanică a produsului Stabilitatea termică a produsului Gust amar 1 lipseşte 2,0 5,5 20 5% prezent puternică înaltă joasă pronunţat 2 1% 3,0 2,0 11 1% absent lipseşte joasă medie slab 3 10% 3,0 5,0 12 lipseşte absent lipseşte satisfăc. înaltă lipseşte 4 5% 4,0 2,5 16 lipseşte absent slabă înaltă înaltă foarte slab№ Tea oil extract Gelatin, % Gelatin, pH Na2SO4 Presence of unencapsulated oil Formation of Na2SO4 sediment Coagulation of the product Mechanical stability of the product Thermal stability of the product Bitter taste 1 absent 2.0 5.5 20 5% present strong high low pronounced 2 1% 3.0 2.0 11 1% absent absent low medium weak 3 10% 3.0 5.0 12 absent absent absent satis. high absent 4 5% 4.0 2.5 16 absent absent weak high high very weak
1. RU 2147923 C1 2000.04.27 1. RU 2147923 C1 2000.04.27
2. RU 2305473 C1 2007.09.10 2. RU 2305473 C1 2007.09.10
3. RU 2316390 C2 2008.02.10 3. RU 2316390 C2 2008.02.10
Claims (3)
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| MDS20120073A MD557Z (en) | 2012-05-11 | 2012-05-11 | Process for microencapsulation of food and cosmetic oil compositions |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| MDS20120073A MD557Z (en) | 2012-05-11 | 2012-05-11 | Process for microencapsulation of food and cosmetic oil compositions |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| MD557Y MD557Y (en) | 2012-11-30 |
| MD557Z true MD557Z (en) | 2013-06-30 |
Family
ID=47296860
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| MDS20120073A MD557Z (en) | 2012-05-11 | 2012-05-11 | Process for microencapsulation of food and cosmetic oil compositions |
Country Status (1)
| Country | Link |
|---|---|
| MD (1) | MD557Z (en) |
Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU509289A1 (en) * | 1973-06-25 | 1976-04-05 | Предприятие П/Я В-8469 | The method of producing microcapsules |
| SU912260A1 (en) * | 1980-05-27 | 1982-03-15 | Украинская Ордена Трудового Красного Знамени Сельскохозяйственная Академия | Microcapsule production method |
| GB2192169A (en) * | 1986-05-26 | 1988-01-06 | Fuji Photo Film Co Ltd | Method of forming polymeric microcapsules containing oily liquid |
| RU2122464C1 (en) * | 1996-09-11 | 1998-11-27 | Ивановский государственный университет | Method of preparing microcapsules |
| RU2147923C1 (en) * | 1997-12-02 | 2000-04-27 | Ивановский государственный университет | Technology of production of microcapsules |
| RU2305473C1 (en) * | 2006-03-07 | 2007-09-10 | Общество с ограниченной ответственностью "Артлайф" | Method for microincapsulation of flavoring substances and flavoring product obtained by using the same |
| RU2316390C2 (en) * | 2005-11-23 | 2008-02-10 | Ставропольский государственный университет | Method of production of the microcapsules |
-
2012
- 2012-05-11 MD MDS20120073A patent/MD557Z/en not_active IP Right Cessation
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU509289A1 (en) * | 1973-06-25 | 1976-04-05 | Предприятие П/Я В-8469 | The method of producing microcapsules |
| SU912260A1 (en) * | 1980-05-27 | 1982-03-15 | Украинская Ордена Трудового Красного Знамени Сельскохозяйственная Академия | Microcapsule production method |
| GB2192169A (en) * | 1986-05-26 | 1988-01-06 | Fuji Photo Film Co Ltd | Method of forming polymeric microcapsules containing oily liquid |
| RU2122464C1 (en) * | 1996-09-11 | 1998-11-27 | Ивановский государственный университет | Method of preparing microcapsules |
| RU2147923C1 (en) * | 1997-12-02 | 2000-04-27 | Ивановский государственный университет | Technology of production of microcapsules |
| RU2316390C2 (en) * | 2005-11-23 | 2008-02-10 | Ставропольский государственный университет | Method of production of the microcapsules |
| RU2305473C1 (en) * | 2006-03-07 | 2007-09-10 | Общество с ограниченной ответственностью "Артлайф" | Method for microincapsulation of flavoring substances and flavoring product obtained by using the same |
Also Published As
| Publication number | Publication date |
|---|---|
| MD557Y (en) | 2012-11-30 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| Matos et al. | Encapsulation of resveratrol using food-grade concentrated double emulsions: Emulsion characterization and rheological behaviour | |
| CN104921047B (en) | Microcapsule mustard essence and preparation method thereof | |
| Martinez et al. | Oxidative stability of walnut (Juglans regia L.) and chia (Salvia hispanica L.) oils microencapsulated by spray drying | |
| Botrel et al. | Application of cashew tree gum on the production and stability of spray-dried fish oil | |
| EP3305084B1 (en) | Capsules containing two phases and method for their preparation | |
| CN105802725B (en) | A kind of preparation method and application of new type functional plant powder grease | |
| CN101564667B (en) | Method for preparing alginate soft capsule | |
| CN109820837A (en) | A kind of microcapsules of the ester containing natural astaxanthin and preparation method thereof | |
| CN102742810A (en) | Garlic oil microcapsule with shell made of soybean protein isolate and chitosan and preparation method and application thereof | |
| Vasile et al. | Prosopis alba exudate gum as novel excipient for fish oil encapsulation in polyelectrolyte bead system | |
| Marcela et al. | Microencapsulation of L-ascorbic acid by spray drying using sodium alginate as wall material | |
| CN106509893A (en) | Essence oil microcapsules and preparation method thereof | |
| CN108125799A (en) | A kind of composite slow release essence microcapsule and preparation method thereof | |
| CN111659328B (en) | Preparation process of linseed oil microcapsule and product thereof | |
| Nurhadi et al. | The virgin coconut oil (VCO) emulsion powder characteristics: effect of pickering emulsion with microcrystalline cellulose (MCC) and different drying techniques. | |
| MD557Z (en) | Process for microencapsulation of food and cosmetic oil compositions | |
| CN107811297A (en) | A kind of setose abelmoschus seed oil microcapsule and preparation method thereof | |
| US2183084A (en) | Method of making activated gelatin | |
| KR101526689B1 (en) | Composition of biopolymer microcapsule and method of preparation | |
| JP6818209B2 (en) | Manufacturing method of external preparations for skin and external preparations for skin | |
| CN103933905A (en) | Prinsepia utilis royle fruit oil microsphere and preparation method thereof | |
| KR100616133B1 (en) | Oil-containing microcapsules manufacturing method | |
| EP3860353B1 (en) | Method for producing a phospholipid concentrate from a dairy composition | |
| CN108774342A (en) | A kind of orange oil pickering emulsion and preparation method thereof stablized using nano-cellulose | |
| CN108623820A (en) | A kind of orange oil pickering emulsion and preparation method thereof stablized using regenerated cellulose |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| FG9Y | Short term patent issued | ||
| MK4Y | Short term patent expired |