MD1782Z - Process for producing natural brown colorant from walnut kernels - Google Patents
Process for producing natural brown colorant from walnut kernels Download PDFInfo
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- MD1782Z MD1782Z MDS20230098A MDS20230098A MD1782Z MD 1782 Z MD1782 Z MD 1782Z MD S20230098 A MDS20230098 A MD S20230098A MD S20230098 A MDS20230098 A MD S20230098A MD 1782 Z MD1782 Z MD 1782Z
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- Moldova
- Prior art keywords
- walnut kernels
- temperature
- dye
- extraction
- ethyl alcohol
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- 235000009496 Juglans regia Nutrition 0.000 title claims abstract description 18
- 235000020234 walnut Nutrition 0.000 title claims abstract description 18
- 238000000034 method Methods 0.000 title claims abstract description 15
- 240000007049 Juglans regia Species 0.000 title description 2
- 239000003086 colorant Substances 0.000 title 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- 241000758789 Juglans Species 0.000 claims abstract description 16
- 235000019441 ethanol Nutrition 0.000 claims abstract description 15
- 238000000605 extraction Methods 0.000 claims abstract description 15
- 239000001049 brown dye Substances 0.000 claims abstract description 13
- 239000000284 extract Substances 0.000 claims abstract description 12
- 239000000243 solution Substances 0.000 claims abstract description 12
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims abstract description 11
- 239000007787 solid Substances 0.000 claims abstract description 11
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims abstract description 6
- 239000006286 aqueous extract Substances 0.000 claims abstract description 5
- 239000001110 calcium chloride Substances 0.000 claims abstract description 4
- 229910001628 calcium chloride Inorganic materials 0.000 claims abstract description 4
- 239000012047 saturated solution Substances 0.000 claims abstract description 4
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 3
- 235000013305 food Nutrition 0.000 abstract description 11
- 239000000975 dye Substances 0.000 description 12
- 239000002994 raw material Substances 0.000 description 6
- 238000004821 distillation Methods 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 241000196324 Embryophyta Species 0.000 description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- 229910000029 sodium carbonate Inorganic materials 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- 108010059820 Polygalacturonase Proteins 0.000 description 2
- CZMRCDWAGMRECN-UHFFFAOYSA-N Rohrzucker Natural products OCC1OC(CO)(OC2OC(CO)C(O)C(O)C2O)C(O)C1O CZMRCDWAGMRECN-UHFFFAOYSA-N 0.000 description 2
- 238000004040 coloring Methods 0.000 description 2
- 235000009508 confectionery Nutrition 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 238000004880 explosion Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 235000014594 pastries Nutrition 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 241000218645 Cedrus Species 0.000 description 1
- 241000758791 Juglandaceae Species 0.000 description 1
- 235000014075 Juglans mandschurica Nutrition 0.000 description 1
- 244000264601 Juglans mandschurica Species 0.000 description 1
- 229930192627 Naphthoquinone Natural products 0.000 description 1
- 229930182559 Natural dye Natural products 0.000 description 1
- 230000001133 acceleration Effects 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 230000001093 anti-cancer Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 235000019463 artificial additive Nutrition 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000012153 distilled water Substances 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 235000013373 food additive Nutrition 0.000 description 1
- 239000002778 food additive Substances 0.000 description 1
- 239000000576 food coloring agent Substances 0.000 description 1
- 239000000989 food dye Substances 0.000 description 1
- 239000010794 food waste Substances 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000000227 grinding Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000003859 lipid peroxidation Effects 0.000 description 1
- 150000002791 naphthoquinones Chemical class 0.000 description 1
- 239000000978 natural dye Substances 0.000 description 1
- 235000016709 nutrition Nutrition 0.000 description 1
- 230000035764 nutrition Effects 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N phenol group Chemical group C1(=CC=CC=C1)O ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000003449 preventive effect Effects 0.000 description 1
- 150000004053 quinones Chemical class 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 230000001256 tonic effect Effects 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
Abstract
Invenţia se referă la industria alimentară, şi anume la un procedeu de obţinere a colorantului natural brun din miez de nuci.Procedeul, conform invenţiei, include extracţia miezului de nuci cu o soluţie ce conţine 25-30% alcool etilic şi 1% carbonat de sodiu anhidru. Extracţia se efectuează timp de 10-15 min, la o temperatură de 40-45°C şi tratare cu ultrasunet cu frecvenţa de 37 MHz. După care din extractul obţinut se distilează alcoolul etilic, iar extractul concentrat apos rezultat se tratează cu soluţie saturată de clorură de calciu pentru separarea colorantului brun în stare solidă, care apoi se usucă.The invention relates to the food industry, namely to a process for obtaining natural brown dye from walnut kernels. The process, according to the invention, includes the extraction of walnut kernels with a solution containing 25-30% ethyl alcohol and 1% anhydrous sodium carbonate. The extraction is carried out for 10-15 min, at a temperature of 40-45°C and ultrasound treatment with a frequency of 37 MHz. After which the ethyl alcohol is distilled from the obtained extract, and the resulting concentrated aqueous extract is treated with a saturated solution of calcium chloride to separate the brown dye in the solid state, which is then dried.
Description
Invenţia se referă la industria alimentară, şi anume la un procedeu de obţinere a colorantului natural brun din miez de nuci. The invention relates to the food industry, namely to a process for obtaining natural brown dye from walnut kernels.
Este cunoscut procedeul de obţinere a colorantului alimentar din coajă de nuci, care prevede extracţia din coaja de nuci sau din septum, sau din coaja de cedru, sau din amestecul acestora. Extracţia se realizează cu o soluţie de alcool etilic cu o concentraţie de 96-98% timp de 2-3 ore, fără tratarea prealabilă a materiilor prime. Extractul se separă de solvent prin distilare în două etape. Prima etapă constă în distilarea alcoolului pentru a obţine un colorant cu o concentraţie de 50%, iar a doua etapă constă în eliminarea completă a alcoolului. Între prima şi a doua etapă de separare a agentului de extracţie de colorant, la concentrat se adaugă zahăr din sfeclă în raport de soluţie de colorant:zahăr din sfeclă egal cu 70:30 [1]. The process of obtaining food coloring from walnut shells is known, which provides for the extraction of walnut shells or septum, or cedar bark, or a mixture thereof. The extraction is carried out with a solution of ethyl alcohol with a concentration of 96-98% for 2-3 hours, without prior treatment of the raw materials. The extract is separated from the solvent by distillation in two stages. The first stage consists of distilling the alcohol to obtain a dye with a concentration of 50%, and the second stage consists of the complete elimination of the alcohol. Between the first and second stages of separation of the dye extraction agent, beet sugar is added to the concentrate in a ratio of dye solution: beet sugar equal to 70:30 [1].
Dezavantajul acestui procedeu constă în durata lungă a extacţiei, necesitatea utilizării alcoolului etilic de înaltă concentraţie ce prezintă pericole de incendiu [Алексеев С. Г., Пищальников А. В., Левковец И. А., Барбин Н. М. О пожароопасности водных растворов этанола. Пожаровзрывобезопасность. 2010, том 19, №5, р. 31-33 ]. Adăugarea zahărului la etapa de separare a colorantului diminuează aria utilizării produsului pentru colorarea diferitor alimente. The disadvantage of this process is the long extraction time, the need to use high-concentration ethyl alcohol, which poses a fire hazard [Alekseev S. G., Pischalnikov A. V., Levkovets I. A., Barbin N. M. On the fire hazard of aqueous solutions of ethanol. Explosion and explosion safety. 2010, vol. 19, no. 5, p. 31-33]. The addition of sugar at the stage of separating the dye reduces the area of use of the product for coloring various foods.
De asemenea este cunoscut un procedeu de obţinere a unui colorant în forma solubilă din materie primă vegetală care prevede uscarea materiei prime vegetale (pericarpul nucilor de Manciuria) până la 105°C timp de 3 ore sau congelarea şi măcinarea acesteia până la o dimensiune care nu depăşeşte 3 mm. Materia primă obţinută se extrage cu apă distilată la temperatura de 100°C şi hidromodul de 1:5, timp de 5 minute. Extractul obţinut se răceşte până la 23°C. Colorantul se separă în formă de filtrat de reziduurile materiei prime vegetale [2]. Also known is a process for obtaining a soluble dye from plant raw material, which involves drying the plant raw material (the pericarp of Manchurian walnuts) at up to 105°C for 3 hours or freezing and grinding it to a size not exceeding 3 mm. The obtained raw material is extracted with distilled water at a temperature of 100°C and a hydromodulus of 1:5, for 5 minutes. The obtained extract is cooled to 23°C. The dye is separated in the form of a filtrate from the residues of the plant raw material [2].
Dezavantajul acestui procedeu constă în necesitatea încălzirii îndelungate sau răcirii profunde, ceea ce duce la cheltuieli mari de energie. Din descrierea procedeului nu este evidentă modalitatea de filtrare şi caracteristicile filtrului utilizat, fiind indicată dimensiunea porilor care depăşeşte mărimea particulelor materiei prime supuse filtrării. The disadvantage of this process is the need for long heating or deep cooling, which leads to high energy costs. The description of the process does not indicate the filtration method and the characteristics of the filter used, indicating the pore size that exceeds the particle size of the raw material being filtered.
Cea mai apropiată soluţie de prezenta invenţie, reprezintă un procedeu de eliminare a compuşilor fenolici şi a naftochinonelor din pieliţa miezului de nuciJuglans regiaL. Procedeul, include extracţia multiplă a miezului de nuci într-un extractor cilindric rotitor, cu un extractant, ce conţine alcool etilic alimentar 7-15% vol., carbonat de sodiu 0,2-0,5%, poligalacturonază 0,02-0,04% şi apă. Extracţia se efectuează la temperatura de 20- 40°C, după care miezul de nuci se spală cu o soluţie de acid citric de 0,5% şi se usucă la aer [3]. The closest solution to the present invention is a process for removing phenolic compounds and naphthoquinones from the skin of the walnut kernel Juglans regia L. The process includes multiple extraction of the walnut kernel in a rotating cylindrical extractor, with an extractant containing 7-15% vol. food ethyl alcohol, 0.2-0.5% sodium carbonate, 0.02-0.04% polygalacturonase and water. The extraction is carried out at a temperature of 20-40°C, after which the walnut kernel is washed with a 0.5% citric acid solution and air-dried [3].
Dezavantajul utilizării acestui procedeu în scopul obţinerii colorantului constă în necesitatea extracţiei multiple, în urma căreia scade concentraţia colorantului în extractul sumar final. Alt dezavantaj este prezenţa enzimei poligalacturonază în compoziţia extractantului. The disadvantage of using this process to obtain the dye is the need for multiple extractions, which reduces the concentration of the dye in the final extract. Another disadvantage is the presence of the enzyme polygalacturonase in the extractant composition.
Protejarea culorii naturale a produselor alimentare prezintă interes şi o necesitate la procesarea alimentelor în industria alimentară. Coloranţii alimentari au un impact important asupra aspectului exterior al alimentelor la restabilirea culorii acestora; de asemenea şi asupra ameliorării calităţilor senzoriale, inofensivităţii şi calităţii produselor alimentare. Protecting the natural color of food products is of interest and a necessity in food processing in the food industry. Food dyes have an important impact on the external appearance of foods by restoring their color; as well as on improving the sensory qualities, harmlessness and quality of food products.
Problema pe care o rezolvă prezenta invenţie, constă în obţinerea colorantului brun natural inofensiv în stare solidă, care poate fi utilizat pentru formarea sau corecţia culorii produselor alimentare. The problem solved by the present invention consists in obtaining a harmless natural brown dye in solid state, which can be used for forming or correcting the color of food products.
Invenţia soluţionează problema prin aceea că se propune un procedeu de obţinere a colorantului natural brun din miez de nuci, care include extracţia miezului de nuci cu o soluţie ce conţine 25-30% alcool etilic şi 1% carbonat de sodiu anhidru, miezul şi soluţia fiind luate într-un raport respectiv de 1:(2-3). The invention solves the problem by proposing a process for obtaining natural brown dye from walnut kernels, which includes extracting the walnut kernels with a solution containing 25-30% ethyl alcohol and 1% anhydrous sodium carbonate, the kernel and the solution being taken in a respective ratio of 1:(2-3).
Extracţia se efectuează timp de 10-15 min, la o temperatură de 40-45°C şi tratare cu ultrasunet cu frecvenţa de 37 MHz. The extraction is carried out for 10-15 min, at a temperature of 40-45°C and ultrasound treatment with a frequency of 37 MHz.
După care, din extractul obţinut se distilează alcoolul etilic la o temperatură de 60-65°C şi presiune de 0,09-0,11 atm, iar extractul concentrat apos rezultat se tratează cu soluţie saturată de clorură de calciu. After which, ethyl alcohol is distilled from the obtained extract at a temperature of 60-65°C and a pressure of 0.09-0.11 atm, and the resulting concentrated aqueous extract is treated with saturated calcium chloride solution.
Ulterior se separă colorantul brun în stare solidă şi se usucă la o temperatură de 60-65°C şi presiune de 0,09-0,11 atm. Subsequently, the brown dye is separated in solid state and dried at a temperature of 60-65°C and a pressure of 0.09-0.11 atm.
Obţinerea unui colorant natural brun la prelucrarea nucilor vechi contribuie la rezolvarea problemei utilizării deşeurilor agroalimentare cu obţinerea de substanţe biologic active (SBA). Datorită efectului antioxidant, tonic, anticancerigen acest colorant poate fi utilizat în alimentaţia medicală şi preventivă, precum şi în producţia de aditivi alimentari biologic activi. În plus, utilizarea acestuia în industria alimentară se datorează capacităţii sale de a inhiba peroxidarea lipidelor, menţinând un timp mai îndelungat caracteristicile organoleptice iniţiale. Cu scopul extinderii gamei de produse fortificate, cu valoare biologică sporită, în absenţa completă a aditivilor sintetici, acest colorant poate fi adăugat la fabricarea dulciurilor şi a produselor de patiserie. Obtaining a natural brown dye from the processing of old walnuts contributes to solving the problem of using agro-food waste to obtain biologically active substances (BAS). Due to its antioxidant, tonic, anticancer effect, this dye can be used in medical and preventive nutrition, as well as in the production of biologically active food additives. In addition, its use in the food industry is due to its ability to inhibit lipid peroxidation, maintaining the initial organoleptic characteristics for a longer time. In order to expand the range of fortified products with increased biological value, in the complete absence of synthetic additives, this dye can be added to the manufacture of sweets and pastries.
Rezultatul invenţiei constă în obţinerea unui colorant natural brun în stare solidă, afânată, care poate fi utilizat pentru colorarea produselor de patiserie şi a dulciurilor. The result of the invention consists in obtaining a brown natural dye in a solid, loose state, which can be used for coloring pastries and sweets.
Argumentarea alegerii parametrilor-cheie ale invenţiei. Justification of the choice of key parameters of the invention.
Extractul care conţine 25-30% alcool este aseptic, nu prezintă pericol înalt de incendii, iar la distilarea ulterioară se asigură evacuarea cantităţilor considerabile de apă cu obţinerea extractului concentrat de colorant. The extract, which contains 25-30% alcohol, is aseptic, does not pose a high fire hazard, and subsequent distillation ensures the evacuation of considerable quantities of water, obtaining the concentrated dye extract.
Soluţia de 1% carbonat de sodiu asigură relaxarea matricei din polimeri care alcătuiesc pieliţa miezului de nuci, respectiv contribuie la extracţia uşoară a coloranţilor. The 1% sodium carbonate solution ensures the relaxation of the polymer matrix that makes up the skin of the walnut kernel, respectively contributing to the easy extraction of dyes.
Ultrasunetul cu frecvenţa de 37 MHz asigură accelerarea şi plenitudinea extracţiei în timp de 10-15 minute, iar temperatura de 40-45°C asigură păstrarea unor compuşi valoroşi atât în extract, cât şi în miezul de nuci. Ultrasound with a frequency of 37 MHz ensures the acceleration and completeness of the extraction within 10-15 minutes, and the temperature of 40-45°C ensures the preservation of valuable compounds both in the extract and in the walnut kernel.
Tratarea cu soluţie saturată de clorură de calciu a extractului concentrat care conţine carbonat de sodiu, asigură separarea colorantului brun în starea solidă, care prezintă compuşi fenolici şi chinonici fixaţi pe matricea solidă de carbonat de calciu. Treatment with saturated calcium chloride solution of the concentrated extract containing sodium carbonate ensures the separation of the brown dye in the solid state, which presents phenolic and quinone compounds fixed on the solid calcium carbonate matrix.
Uscarea colorantului brun în starea solidă la temperatura de 60-65°C şi presiunea de 0,09-0,11 atm asigură evacuarea completă a apei şi obţinerea produsului în formă de pulbere solidă afânată. Drying the brown dye in the solid state at a temperature of 60-65°C and a pressure of 0.09-0.11 atm ensures complete removal of water and obtaining the product in the form of a loose solid powder.
Exemple de realizare a procedeului. Examples of the process.
Exemplul 1 Example 1
La 150 g de miez de nuci se adaugă 300 g soluţie care conţine 30% alcool etilic şi 1% carbonat de sodiu anhidru. Extracţia are loc la 45°C în baia cu ultrasunet, reglată la 37 MHz timp de 10 min. Extractul obţinut se distilează la temperatura de 60°C, presiunea de 0,09 atm până la încetarea procesului de distilare în condiţiile indicate. Extractul concentrat apos obţinut se tratează cu soluţie saturată de clorură de calciu. În rezultat se formează un colorant brun în stare solidă. Acesta se usucă la temperatura de 60°C, presiunea de 0,09 atm până la obţinerea unei pulberi brune afânate. To 150 g of walnut kernels, 300 g of a solution containing 30% ethyl alcohol and 1% anhydrous sodium carbonate are added. The extraction takes place at 45°C in an ultrasonic bath, set at 37 MHz for 10 min. The extract obtained is distilled at a temperature of 60°C, a pressure of 0.09 atm until the distillation process stops under the indicated conditions. The concentrated aqueous extract obtained is treated with a saturated solution of calcium chloride. As a result, a brown dye is formed in the solid state. This is dried at a temperature of 60°C, a pressure of 0.09 atm until a loose brown powder is obtained.
Exemplul 2 Example 2
La 200 grame de miez de nuci se adaugă 600 g soluţie care conţine 25% alcool etilic şi 1% carbonat de sodiu anhidru. Extracţia are loc la 40°C în baia cu ultrasunet, reglată la 37 MHz timp de 15 min. Extractul obţinut se distilează la temperatura de 65°C, presiunea de 0,11 atm până la încetarea procesului de distilare în condiţiile indicate. Extractul concentrat apos obţinut se tratează cu soluţie saturată de clorură de calciu. În rezultat se formează un colorant brun în stare solidă. Acesta se usucă la temperatura de 65°C, presiunea de 0,11 atm până la obţinerea unei pulberi brune afânate. To 200 grams of walnut kernels, 600 g of a solution containing 25% ethyl alcohol and 1% anhydrous sodium carbonate are added. The extraction takes place at 40°C in an ultrasonic bath, set at 37 MHz for 15 min. The extract obtained is distilled at a temperature of 65°C, a pressure of 0.11 atm until the distillation process stops under the indicated conditions. The concentrated aqueous extract obtained is treated with a saturated solution of calcium chloride. As a result, a brown dye is formed in the solid state. This is dried at a temperature of 65°C, a pressure of 0.11 atm until a loose brown powder is obtained.
1. RU 2287540 C2 2006.11.20 1. RU 2287540 C2 2006.11.20
2. RU 2601452 C2 2016.11.10 2. RU 2601452 C2 2016.11.10
3. MD 1566 Y 2021.10.31 3. MD 1566 Y 2021.10.31
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