RU2624532C1 - Method of obtaining chia seeds nanocapules (salvia hispanica) in konjac gum - Google Patents
Method of obtaining chia seeds nanocapules (salvia hispanica) in konjac gum Download PDFInfo
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- RU2624532C1 RU2624532C1 RU2016109424A RU2016109424A RU2624532C1 RU 2624532 C1 RU2624532 C1 RU 2624532C1 RU 2016109424 A RU2016109424 A RU 2016109424A RU 2016109424 A RU2016109424 A RU 2016109424A RU 2624532 C1 RU2624532 C1 RU 2624532C1
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- 235000020235 chia seed Nutrition 0.000 title claims abstract description 13
- 229920002752 Konjac Polymers 0.000 title claims abstract description 10
- 239000000252 konjac Substances 0.000 title claims abstract description 10
- 235000019823 konjac gum Nutrition 0.000 title claims abstract description 10
- 238000000034 method Methods 0.000 title claims description 16
- 240000005481 Salvia hispanica Species 0.000 title 1
- 235000001498 Salvia hispanica Nutrition 0.000 title 1
- 239000002088 nanocapsule Substances 0.000 claims abstract description 15
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 8
- VFWCMGCRMGJXDK-UHFFFAOYSA-N 1-chlorobutane Chemical compound CCCCCl VFWCMGCRMGJXDK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000001793 Citric acid esters of mono and diglycerides of fatty acids Substances 0.000 claims abstract description 4
- 239000000843 powder Substances 0.000 claims abstract description 4
- 239000004094 surface-active agent Substances 0.000 claims abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 3
- 230000000694 effects Effects 0.000 abstract description 2
- 230000001133 acceleration Effects 0.000 abstract 1
- 239000000126 substance Substances 0.000 abstract 1
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 6
- 239000003094 microcapsule Substances 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 4
- 239000007921 spray Substances 0.000 description 4
- 238000005259 measurement Methods 0.000 description 3
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerol Natural products OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 description 2
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 235000014113 dietary fatty acids Nutrition 0.000 description 2
- 238000010790 dilution Methods 0.000 description 2
- 239000012895 dilution Substances 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 239000000194 fatty acid Substances 0.000 description 2
- 229930195729 fatty acid Natural products 0.000 description 2
- 150000004665 fatty acids Chemical class 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 239000002105 nanoparticle Substances 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000001556 precipitation Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000003756 stirring Methods 0.000 description 2
- 206010067484 Adverse reaction Diseases 0.000 description 1
- 239000004135 Bone phosphate Substances 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 102220547770 Inducible T-cell costimulator_A23L_mutation Human genes 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000004480 active ingredient Substances 0.000 description 1
- 230000006838 adverse reaction Effects 0.000 description 1
- 239000012736 aqueous medium Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 125000005456 glyceride group Chemical group 0.000 description 1
- -1 glycerol ester Chemical class 0.000 description 1
- 239000002917 insecticide Substances 0.000 description 1
- 150000004715 keto acids Chemical class 0.000 description 1
- 150000002632 lipids Chemical class 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 102000004169 proteins and genes Human genes 0.000 description 1
- 108090000623 proteins and genes Proteins 0.000 description 1
- 239000002728 pyrethroid Substances 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 229920003169 water-soluble polymer Polymers 0.000 description 1
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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
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5192—Processes
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF
- A23L25/00—Food consisting mainly of nutmeat or seeds; Preparation or treatment thereof
- A23L25/20—Food consisting mainly of nutmeat or seeds; Preparation or treatment thereof consisting of whole seeds or seed fragments
- A23L25/25—Food consisting mainly of nutmeat or seeds; Preparation or treatment thereof consisting of whole seeds or seed fragments coated with a layer
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61J—CONTAINERS SPECIALLY ADAPTED FOR MEDICAL OR PHARMACEUTICAL PURPOSES; DEVICES OR METHODS SPECIALLY ADAPTED FOR BRINGING PHARMACEUTICAL PRODUCTS INTO PARTICULAR PHYSICAL OR ADMINISTERING FORMS; DEVICES FOR ADMINISTERING FOOD OR MEDICINES ORALLY; BABY COMFORTERS; DEVICES FOR RECEIVING SPITTLE
- A61J3/00—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms
- A61J3/07—Devices or methods specially adapted for bringing pharmaceutical products into particular physical or administering forms into the form of capsules or similar small containers for oral use
-
- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61K—PREPARATIONS FOR MEDICAL, DENTAL OR TOILETRY PURPOSES
- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
- A61K36/18—Magnoliophyta (angiosperms)
- A61K36/185—Magnoliopsida (dicotyledons)
- A61K36/53—Lamiaceae or Labiatae (Mint family), e.g. thyme, rosemary or lavender
- A61K36/537—Salvia (sage)
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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
- A61K9/51—Nanocapsules; Nanoparticles
- A61K9/5107—Excipients; Inactive ingredients
- A61K9/513—Organic macromolecular compounds; Dendrimers
- A61K9/5161—Polysaccharides, e.g. alginate, chitosan, cellulose derivatives; Cyclodextrin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y5/00—Nanobiotechnology or nanomedicine, e.g. protein engineering or drug delivery
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Abstract
Description
Изобретение относится к области нанотехнологии и пищевой промышленности.The invention relates to the field of nanotechnology and the food industry.
Ранее были известны способы получения микрокапсул.Previously known methods for producing microcapsules.
В пат. 2173140, МПК А61K 009/50, А61K 009/127, Российская Федерация, опубликован 10.09.2001, предложен способ получения кремнийорганолипидных микрокапсул с использованием роторно-кавитационной установки, обладающей высокими сдвиговыми усилиями и мощными гидроакустическими явлениями звукового и ультразвукового диапазона для диспергирования.In US Pat. 2173140, IPC A61K 009/50, A61K 009/127, Russian Federation, published September 10, 2001. A method for producing silicon organolipid microcapsules using a rotary-cavitation unit with high shear forces and powerful sonar acoustic and ultrasonic dispersion ranges is proposed.
Недостатком данного способа является применение специального оборудования - роторно-кавитационной установки, которая обладает ультразвуковым действием, что оказывает влияние на образование микрокапсул и при этом может вызывать побочные реакции в связи с тем, что ультразвук разрушающе действует на полимеры белковой природы, поэтому предложенный способ применим при работе с полимерами синтетического происхожденияThe disadvantage of this method is the use of special equipment - a rotary cavitation unit, which has an ultrasonic effect, which affects the formation of microcapsules and can cause adverse reactions due to the fact that ultrasound destructively affects polymers of a protein nature, therefore, the proposed method is applicable when work with polymers of synthetic origin
В пат. 2359662, МПК А61K 009/56, A61J 003/07, B01J 013/02, A23L 001/00, опубликован 27.06.2009, Российская Федерация, предложен способ получения микрокапсул хлорида натрия с использованием распылительного охлаждения в распылительной градирне Niro при следующих условиях: температура воздуха на входе 10°С, температура воздуха на выходе 28°С, скорость вращения распыляющего барабана 10000 оборотов/мин. Микрокапсулы по изобретению обладают улучшенной стабильностью и обеспечивают регулируемое и/или пролонгированное высвобождение активного ингредиента.In US Pat. 2359662, IPC A61K 009/56, A61J 003/07, B01J 013/02, A23L 001/00, published June 27, 2009, Russian Federation, a method for producing sodium chloride microcapsules using spray cooling in a Niro spray cooling tower under the following conditions: temperature air inlet 10 ° C, air outlet temperature 28 ° C, the rotation speed of the spray drum 10,000 rpm. The microcapsules of the invention have improved stability and provide controlled and / or prolonged release of the active ingredient.
Недостатками предложенного способа являются длительность процесса и применение специального оборудования, комплекс определенных условий (температура воздуха на входе 10°С, температура воздуха на выходе 28°С, скорость вращения распыляющего барабана 10000 оборотов/мин).The disadvantages of the proposed method are the duration of the process and the use of special equipment, a set of certain conditions (air temperature at the inlet 10 ° C, air temperature at the outlet 28 ° C, rotation speed of the spray drum 10,000 rpm).
Наиболее близким методом является способ, предложенный в пат. 2134967, МПК A01N 53/00, A01N 25/28, опубликован 27.08.1999, Российская Федерация (1999). В воде диспергируют раствор смеси природных липидов и пиретроидного инсектицида в весовом отношении 2-4:1 в органическом растворителе, что приводит к упрощению способа микрокапсулирования.The closest method is the method proposed in US Pat. 2134967, IPC A01N 53/00, A01N 25/28, published on 08.27.1999, Russian Federation (1999). A solution of a mixture of natural lipids and a pyrethroid insecticide in a weight ratio of 2-4: 1 in an organic solvent is dispersed in water, which simplifies the microencapsulation method.
Недостатком метода является диспергирование в водной среде, что делает предложенный способ неприменимым для получения микрокапсул водорастворимых препаратов в водорастворимых полимерах.The disadvantage of this method is dispersion in an aqueous medium, which makes the proposed method inapplicable for producing microcapsules of water-soluble preparations in water-soluble polymers.
Техническая задача - упрощение и ускорение процесса получения нанокапсул, уменьшение потерь при получении нанокапсул (увеличение выхода по массе).The technical task is to simplify and accelerate the process of obtaining nanocapsules, reduce losses in obtaining nanocapsules (increase in yield by mass).
Решение технической задачи достигается способом получения нанокапсул семян чиа, отличающимся тем, что в качестве оболочки нанокапсул используется конжаковая камедь, а в качестве ядра - семена чиа при получении нанокапсул методом осаждения нерастворителем с применением бутилхлорида в качестве осадителя.The solution to the technical problem is achieved by the method of producing nanocapsules of chia seeds, characterized in that konjac gum is used as the shell of the nanocapsules, and chia seeds are used as the core when nanocapsules are prepared by non-solvent precipitation using butyl chloride as a precipitant.
Отличительной особенностью предлагаемого метода является получение нанокапсул методом осаждения нерастворителем с использованием бутилхлорида в качестве осадителя, а также использование конжаковой камеди в качестве оболочки частиц и семян чиа - в качестве ядра.A distinctive feature of the proposed method is the preparation of nanocapsules by non-solvent precipitation using butyl chloride as a precipitant, as well as the use of konjac gum as a shell of particles and chia seeds as a core.
На рис. 1 изображены распределение частиц по размерам в образце нанокапсул семян чиа в конжаковой камеди (соотношение ядро:оболочка 1:3) и статистические характеристики распределений.In fig. Figure 1 shows the particle size distribution in the sample of chia seed nanocapsules in konjac gum (core: shell ratio 1: 3) and statistical characteristics of the distributions.
ПРИМЕР 1. Получение нанокапсул семян чиа в соотношении ядро:оболочка 1:1EXAMPLE 1. Obtaining nanocapsules of chia seeds in the ratio of core: shell 1: 1
1 г порошкообразного семян чиа медленно добавляют в суспензию 1 г конжаковой камеди в бензоле в присутствии 0,01 г препарата Е472с (сложный эфир глицерина с одной-двумя молекулами пищевых жирных кислот и одной-двумя молекулами лимонной кислоты, причем лимонная кислота, как трехосновная, может быть этерифицирована другими глицеридами и как оксокислота - другими жирными кислотами). Свободные кислотные группы могут быть нейтрализованы натрием) в качестве поверхностно-активного вещества при перемешивании 1000 об/мин. Далее приливают 6 мл бутилхлорида. Полученную суспензию отфильтровывают и сушат при комнатной температуре.1 g of powdered chia seeds is slowly added to a suspension of 1 g of konjac gum in benzene in the presence of 0.01 g of the preparation E472c (glycerol ester with one or two molecules of food fatty acids and one or two molecules of citric acid, with citric acid as a tribasic, can be esterified with other glycerides and as an oxo acid with other fatty acids). Free acid groups can be neutralized with sodium) as a surfactant with stirring at 1000 rpm. Next, 6 ml of butyl chloride are added. The resulting suspension is filtered and dried at room temperature.
Получено 2 г порошка нанокапсул. Выход составил 100%.Received 2 g of nanocapsule powder. The yield was 100%.
ПРИМЕР 2. Получение нанокапсул семян чиа в соотношении ядро:оболочка 1:3EXAMPLE 2. Obtaining nanocapsules of chia seeds in the ratio of core: shell 1: 3
1 г порошкообразного семян чиа медленно добавляют в суспензию 3 г конжаковой камеди в бензоле в присутствии 0,01 г препарата Е472с в качестве поверхностно-активного вещества при перемешивании 1000 об/мин. Далее приливают 8 мл бутилхлорида. Полученную суспензию отфильтровывают и сушат при комнатной температуре.1 g of powdered chia seeds is slowly added to a suspension of 3 g of konjac gum in benzene in the presence of 0.01 g of the preparation E472c as a surfactant with stirring at 1000 rpm. Next, 8 ml of butyl chloride are added. The resulting suspension is filtered and dried at room temperature.
Получено 4 г порошка нанокапсул. Выход составил 100%.Received 4 g of nanocapsule powder. The yield was 100%.
ПРИМЕР 3. Определение размеров нанокапсул методом NTAEXAMPLE 3. Determination of the size of nanocapsules by NTA
Измерения проводили на мультипараметрическом анализаторе наночастиц Nanosight LM0 производства Nanosight Ltd (Великобритания) в конфигурации HS-BF (высокочувствительная видеокамера Andor Luca, полупроводниковый лазер с длиной волны 405 нм и мощностью 45 мВт).The measurements were carried out on a Nanosight LM0 multiparameter nanoparticle analyzer manufactured by Nanosight Ltd (Great Britain) in the HS-BF configuration (Andor Luca high-sensitivity video camera, 405 nm semiconductor laser with a power of 45 mW).
Прибор основан на методе анализа траекторий наночастиц (Nanoparticle Tracking Analysis, NTA), описанном в ASTM E2834.The device is based on the Nanoparticle Tracking Analysis (NTA) method described in ASTM E2834.
Оптимальным разведением для разведения было выбрано 1:100. Для измерения были выбраны параметры прибора: Camera Level = 16, Detection Threshold = 10 (multi), Min Track Length:Auto, Min Expected Size: Auto. длительность единичного измерения 215s, использование шприцевого насоса.The optimal dilution for dilution was 1: 100. For the measurement, the device parameters were selected: Camera Level = 16, Detection Threshold = 10 (multi), Min Track Length: Auto, Min Expected Size: Auto. duration of a single measurement of 215s, the use of a syringe pump.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2659394C1 (en) * | 2017-11-10 | 2018-07-02 | Александр Александрович Кролевец | Method of production of bread containing nanostructured chia seeds |
| RU2669292C1 (en) * | 2017-11-10 | 2018-10-09 | Александр Александрович Кролевец | Method for production of ice cream with nanostructured chia seeds |
| RU2718828C1 (en) * | 2019-01-17 | 2020-04-14 | Татьяна Николаевна Алексеева | Alcohol-free beverage |
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| US20090252758A1 (en) * | 2008-04-07 | 2009-10-08 | Mazed Mohammad A | Nutritional supplement for the prevention of cardiovascular disease, alzheimer's disease, diabetes, and regulation and reduction of blood sugar and insulin resistance |
| RU2554763C1 (en) * | 2014-03-26 | 2015-06-27 | Александр Александрович Кролевец | Method of obtaining nanocapsules of chondroitin sulphate in konjac gum |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20090252758A1 (en) * | 2008-04-07 | 2009-10-08 | Mazed Mohammad A | Nutritional supplement for the prevention of cardiovascular disease, alzheimer's disease, diabetes, and regulation and reduction of blood sugar and insulin resistance |
| RU2554763C1 (en) * | 2014-03-26 | 2015-06-27 | Александр Александрович Кролевец | Method of obtaining nanocapsules of chondroitin sulphate in konjac gum |
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| Title |
|---|
| NAGAVARMA B. V. N. Different techniques for preparation of polymeric nanoparticles. Asian Journal Pharm Clin Res, vol.5, suppl 3, 2012, стр.16-23. СОЛОДОВНИК В. Д. Микрокапсулирование. 1980, стр.136-137. * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| RU2659394C1 (en) * | 2017-11-10 | 2018-07-02 | Александр Александрович Кролевец | Method of production of bread containing nanostructured chia seeds |
| RU2669292C1 (en) * | 2017-11-10 | 2018-10-09 | Александр Александрович Кролевец | Method for production of ice cream with nanostructured chia seeds |
| RU2718828C1 (en) * | 2019-01-17 | 2020-04-14 | Татьяна Николаевна Алексеева | Alcohol-free beverage |
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