CN109645426A - A kind of coenzyme, which helps, extracts numb-taste components method - Google Patents
A kind of coenzyme, which helps, extracts numb-taste components method Download PDFInfo
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- CN109645426A CN109645426A CN201811564104.XA CN201811564104A CN109645426A CN 109645426 A CN109645426 A CN 109645426A CN 201811564104 A CN201811564104 A CN 201811564104A CN 109645426 A CN109645426 A CN 109645426A
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- 238000000034 method Methods 0.000 title claims abstract description 19
- 239000000284 extract Substances 0.000 title claims abstract description 16
- -1 which helps Substances 0.000 title description 4
- 239000005515 coenzyme Substances 0.000 title description 3
- 108090000790 Enzymes Proteins 0.000 claims abstract description 53
- 102000004190 Enzymes Human genes 0.000 claims abstract description 53
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 241000949456 Zanthoxylum Species 0.000 claims abstract description 29
- 235000007650 Aralia spinosa Nutrition 0.000 claims abstract description 28
- 238000000605 extraction Methods 0.000 claims abstract description 24
- 239000007788 liquid Substances 0.000 claims abstract description 21
- 230000009514 concussion Effects 0.000 claims abstract description 15
- 239000000287 crude extract Substances 0.000 claims abstract description 11
- 239000012535 impurity Substances 0.000 claims abstract description 9
- 239000011347 resin Substances 0.000 claims abstract description 9
- 229920005989 resin Polymers 0.000 claims abstract description 9
- 239000012153 distilled water Substances 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 8
- 235000013399 edible fruits Nutrition 0.000 claims abstract description 4
- 238000005119 centrifugation Methods 0.000 claims abstract description 3
- 229940088598 enzyme Drugs 0.000 claims description 48
- 244000089698 Zanthoxylum simulans Species 0.000 claims description 27
- 238000004064 recycling Methods 0.000 claims description 16
- 239000006228 supernatant Substances 0.000 claims description 16
- 108010059892 Cellulase Proteins 0.000 claims description 15
- 229940106157 cellulase Drugs 0.000 claims description 15
- 229940059442 hemicellulase Drugs 0.000 claims description 13
- 108010002430 hemicellulase Proteins 0.000 claims description 13
- 230000007062 hydrolysis Effects 0.000 claims description 9
- 238000006460 hydrolysis reaction Methods 0.000 claims description 9
- 239000002994 raw material Substances 0.000 claims description 9
- 235000008534 Capsicum annuum var annuum Nutrition 0.000 claims description 8
- 240000008384 Capsicum annuum var. annuum Species 0.000 claims description 8
- 238000004587 chromatography analysis Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000001179 sorption measurement Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 7
- 241000345998 Calamus manan Species 0.000 claims description 6
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 6
- 239000000203 mixture Substances 0.000 claims description 6
- 235000012950 rattan cane Nutrition 0.000 claims description 6
- 238000000638 solvent extraction Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims 7
- 239000003292 glue Substances 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract description 9
- PSKIOIDCXFHNJA-UHFFFAOYSA-N Sanshool Natural products CC=CC=CC=CCCC=CC=CC(=O)NC(C)C PSKIOIDCXFHNJA-UHFFFAOYSA-N 0.000 abstract description 8
- 238000011084 recovery Methods 0.000 abstract description 8
- 229920001144 Hydroxy alpha sanshool Polymers 0.000 abstract description 6
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- 230000014860 sensory perception of taste Effects 0.000 abstract description 3
- 239000000843 powder Substances 0.000 abstract description 2
- 241001079064 Zanthoxylum schinifolium Species 0.000 abstract 1
- 238000000746 purification Methods 0.000 abstract 1
- 238000007873 sieving Methods 0.000 abstract 1
- 230000002255 enzymatic effect Effects 0.000 description 14
- 239000000835 fiber Substances 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 12
- 235000013305 food Nutrition 0.000 description 7
- 238000002474 experimental method Methods 0.000 description 6
- 238000003825 pressing Methods 0.000 description 6
- 238000013461 design Methods 0.000 description 5
- 150000001408 amides Chemical class 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 4
- 239000000047 product Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 230000000638 stimulation Effects 0.000 description 3
- SBXYHCVXUCYYJT-UEOYEZOQSA-N alpha-Sanshool Chemical compound C\C=C\C=C\C=C/CC\C=C\C(=O)NCC(C)C SBXYHCVXUCYYJT-UEOYEZOQSA-N 0.000 description 2
- 210000002421 cell wall Anatomy 0.000 description 2
- 239000003205 fragrance Substances 0.000 description 2
- 230000003301 hydrolyzing effect Effects 0.000 description 2
- 238000005457 optimization Methods 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 108090000604 Hydrolases Proteins 0.000 description 1
- 102000004157 Hydrolases Human genes 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- SBXYHCVXUCYYJT-UMYNZBAMSA-N beta-sanshool Chemical compound C\C=C\C=C\C=C\CC\C=C\C(=O)NCC(C)C SBXYHCVXUCYYJT-UMYNZBAMSA-N 0.000 description 1
- 235000013409 condiments Nutrition 0.000 description 1
- 239000000470 constituent Substances 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 238000013401 experimental design Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 230000006870 function Effects 0.000 description 1
- KVUKDCFEXVWYBN-UHFFFAOYSA-N gamma-sanshooel Natural products CC=CC=CC=CCCC=CC=CC(=O)NCC(C)C KVUKDCFEXVWYBN-UHFFFAOYSA-N 0.000 description 1
- 235000015220 hamburgers Nutrition 0.000 description 1
- 238000004128 high performance liquid chromatography Methods 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 210000000214 mouth Anatomy 0.000 description 1
- 210000005036 nerve Anatomy 0.000 description 1
- 208000035824 paresthesia Diseases 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000194 supercritical-fluid extraction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/14—Dried spices
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L27/00—Spices; Flavouring agents or condiments; Artificial sweetening agents; Table salts; Dietetic salt substitutes; Preparation or treatment thereof
- A23L27/10—Natural spices, flavouring agents or condiments; Extracts thereof
- A23L27/11—Natural spices, flavouring agents or condiments; Extracts thereof obtained by solvent extraction
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23L—FOODS, FOODSTUFFS, OR NON-ALCOHOLIC BEVERAGES, NOT COVERED BY SUBCLASSES A21D OR A23B-A23J; THEIR PREPARATION OR TREATMENT, e.g. COOKING, MODIFICATION OF NUTRITIVE QUALITIES, PHYSICAL TREATMENT; PRESERVATION OF FOODS OR FOODSTUFFS, IN GENERAL
- A23L29/00—Foods or foodstuffs containing additives; Preparation or treatment thereof
- A23L29/06—Enzymes
-
- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23V—INDEXING SCHEME RELATING TO FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES AND LACTIC OR PROPIONIC ACID BACTERIA USED IN FOODSTUFFS OR FOOD PREPARATION
- A23V2002/00—Food compositions, function of food ingredients or processes for food or foodstuffs
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- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Nutrition Science (AREA)
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Food Science & Technology (AREA)
- Polymers & Plastics (AREA)
- Microbiology (AREA)
- Preparation Of Fruits And Vegetables (AREA)
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Medicines Containing Plant Substances (AREA)
Abstract
The invention discloses a kind of methods of enzyme assisted extraction numb-taste components, after the dry broken sieving of Chinese prickly ash fruit peel powder, the enzyme of distilled water and Pricklyash peel quality 2-2.5% is added by solid-liquid ratio 1:10-15(w:v), concussion is added complex enzyme after cultivating and is digested, after press Pricklyash peel solid-liquid ratio 1:10-15(w:v) be added edible alcohol concussion extract, it filters, be evaporated, obtain numb-taste components crude extract;Spicy components primary extract, centrifugation removal of impurities, purification with macroreticular resin and collection spicy components fraction are redissolved with edible alcohol again.Present invention optimizes enzyme class, enzyme additive amount, the parameters for cultivating time and temperature, finally obtain the numb-taste components that recovery rate is 7.6-12.2%, and including fagaramides substances such as OH- ε-sanshool, OH- α-sanshool and OH- β-sanshools, purity reaches 90-92%, and numb sense of taste feels significant.
Description
Technical field
The present invention relates to production of condiments manufacture fields, and in particular to a kind of enzyme assisted extraction numb-taste components method.
Background technique
Chinese prickly ash is a kind of traditional flavouring of China, deep always to be liked by people.In the river of one of Chinese eight big cuisines
It is most widely used in dish.Sichuan cuisine is famous with spicy characteristic, and wherein numb taste source is exactly Chinese prickly ash.By studying hair for a long time
Existing, there is Chinese prickly ash numb taste stimulation and the unsaturated acyl amine substance contained by it to have direct relation.These unsaturated acyl amine substances
Can make one to generate by nerve in stimulation periglottis and oral cavity it is numb feel and tingling sensation, and be referred to as these and feel and be
" fiber crops ".Presently found Chinese prickly ash unsaturated amides substance have α-sanshool, β-sanshool, OH- ε-sanshool, OH- α-sanshool,
Ten many kinds of substance such as OH- β-sanshool, OH- γ-sanshool, OH- γ-different sanshool and OH- ζ-sanshool.
In the food industry, the numb taste characteristic of Chinese prickly ash is pursued by people always, and more and more food will just be assigned fiber crops
Taste characteristic.It is popular at present to have hamburger of rattan green pepper taste and chicken wings, rattan green pepper in KFC by the food of main characteristics of numb taste
Taste grilled fish and rattan green pepper taste string string etc..Therefore, it can be seen that Chinese prickly ash fiber crops taste Speciality Foods have extensively in following food service industry
Application prospect.But with facilitation, the arrival of digitlization and automated production mode, with Pericarpium Zanthoxyli fruit sheet as numb taste
The application that material carrier is added in food system is not able to satisfy the requirement of industrial mass production more and more.People are urgent
A kind of pure spicy components product is needed, and its numb taste degree digitlization fast and accurately can quantitatively be prepared to reach
The food of different fiber crops taste degree.
Enzyme auxiliary extraction technology is by the hydrolysis of enzyme come brokenization eucaryotic cell structure, to discharge more target products
It to increase recovery rate, therefore is a kind of convenience, the credible extractive technique of green of safety.201010615194.8 disclosing a kind of flower
The extracting process of green pepper effective component, comprising the following steps: (a) feedstock processing: Pericarpium Zanthoxyli fruit is digested in closed container
Then broken wall crushes at low temperature;(b) the extraction separation of Chinese prickly ash fragrance component: zanthoxylum powder is added in extraction kettle and uses CO2Extraction
It takes;After sequentially enter extraction-container one and extraction-container two, the pressure of extraction-container one is that 10-12MPa is parsed;(c) Chinese prickly ash fiber crops taste
The extraction of ingredient separates: then slowly increasing the parameter of extraction, while entrainer is added to extraction kettle, collect Chinese prickly ash fiber crops taste
Element.Although more in the invention using the hydrolysis of enzyme come effective component in assisted extraction Chinese prickly ash in foregoing invention
Supercritical CO is focused on2The extraction and separation of technology do not carry out the optimization of detailed research and technological parameter to enzymatic treatment.
In the technology of existing enzyme assisted extraction numb-taste components, scientific worker focuses on mostly is using other technologies
Main extracting method (such as supercritical fluid extraction), and only using enzyme as a kind of pretreatment of raw material means, therefore not to enzyme
Processing carries out detailed research and parameter optimization.
Summary of the invention
In view of above-mentioned shortcoming, the purpose of the present invention is to provide a kind of enzyme assisted extraction numb-taste components method,
Research influences an important factor for enzymatic treatment, including enzyme class, enzyme additive amount, cultivation time, temperature and pH, to obtain a kind of high
The method of enzymatically treating of the extraction numb-taste components of effect.
In order to achieve the above object, the invention adopts the following technical scheme:
A kind of method that coenzyme helps extraction numb-taste components, includes the following steps:
(1) pretreatment of raw material: dry Chinese prickly ash pericarp is crushed using pulverizer, sieve 40-60 mesh is crossed, it is standby to obtain Pricklyash peel
With;
(2) enzyme hydrolysis is handled: weighing Pricklyash peel by solid-liquid ratio 1:10-15(w:v) and distilled water is added, and Pricklyash peel matter is added
The enzyme of 2-2.5% is measured, control temperature, time, pH value carry out concussion cultivation, it is spare to obtain Pricklyash peel enzymolysis liquid;
(3) solvent extraction: by Pricklyash peel enzymolysis liquid press solid-liquid ratio 1:10-15(w:v) be added edible alcohol, control temperature, when
Between shake extract, filtered after to be extracted, collect filtrate, be evaporated recycling edible alcohol, it is standby to obtain numb-taste components crude extract
With;
(4) spicy components purify: redissolving numb-taste components crude extract using edible alcohol, and are centrifuged off solid impurity, receive
Collect supernatant, supernatant is passed through in macroporous adsorption resin chromatography column, collects spicy components fraction, be finally evaporated recycling edible wine
Essence obtains a kind of numb-taste components.
Further, the Chinese prickly ash pericarp is selected from one of pericarpium zanthoxyli bungeani, rattan green pepper or pericarpium zanthoxyli schinifolii.
Further, be 2.5-3h controlled at 40-45 DEG C, control time in the step (2), control pH value is
4.5-5.5。
Further, the enzyme is made of cellulase, hemicellulase and pectase 3:2:1 in mass ratio.
Further, the enzyme can also be made of cellulase, hemicellulase and pectase 2:1:1 in mass ratio.
It further, is 3-3.5h controlled at 50-60 DEG C, control time in the step (3).
Further, centrifugal condition is 4000-5000r/min, centrifugation time 5-10min in the step (4).
Further, the regulation of the pH value is adjusted with the citric acid of 10mg/ml.
The invention also discloses a kind of using numb-taste components made from the above method.
The present invention has the advantages that compared with existing extracting method
(1) selection of enzyme class is vital for enzymatic treatment.The present invention is by experiment of single factor from numerous hydrolases
It is cellulase, hemicellulase and pectase respectively it is preferred that going out 3 kinds of enzymes with good hydrolytic Chinese prickly ash cell wall.And lead to
Synergistic effect of the mixing experimental study between them is crossed, discovery ratio synergy in 3:2:1 and 2:1:1 is best.Therefore, it obtains
A kind of enzyme ratio with excellent hydrolytic Chinese prickly ash cell wall effect is arrived.
(2) factor for influencing enzymatic treatment effect study and optimize using the experiment of system in the present invention, therefrom
It was found that influencing the principal element of enzymatic treatment, including enzyme class, enzyme additive amount, cultivation time and temperature.To its technological parameter
It is optimized, finally obtaining numb-taste components (pericarpium zanthoxyli bungeani, rattan green pepper and pericarpium zanthoxyli schinifolii) recovery rate is 7.6-12.2%, than general
Extracting method (2.0-8.9%) it is much higher.
(3) present invention assists edible alcohol extraction by enzyme, has obtained a kind of yellow or yellow green and has had Chinese prickly ash fragrance
Medicinal extract shape fluid.By subsequent further efficient liquid phase detection discovery, in numb-taste components there are OH- ε-sanshool,
Fagaramides substance, the purity such as OH- α-sanshool and OH- β-sanshool reach 90-92%.Therefore illustrate, the present invention, which extracts, to be produced
Object spicy components purity is high, numb sense of taste feel significant, are a kind of preferable numb-taste components extracts of quality.
Detailed description of the invention
Fig. 1 is that pericarpium zanthoxyli bungeani spicy components HPLC detects amide substance type;
Fig. 2 is Chinese prickly ash residue electron-microscope scanning figure in embodiment 1;
Fig. 3 is Chinese prickly ash residue electron-microscope scanning figure in embodiment 2;
Fig. 4 is Chinese prickly ash residue electron-microscope scanning figure in embodiment 3;
Fig. 5 is Chinese prickly ash residue electron-microscope scanning figure in comparative example 1;
Fig. 6 is Chinese prickly ash residue electron-microscope scanning figure in comparative example 2;
Fig. 7 is Chinese prickly ash residue electron-microscope scanning figure in comparative example 3.
Specific embodiment
The present invention is specifically described below by embodiment and comparative example, it is necessary to which indicated herein is following reality
It applies example and is served only for that invention is further explained, should not be understood as limiting the scope of the invention.The skill in the field
Art skilled person can make some nonessential modifications and adaptations to the present invention according to the content of aforementioned present invention.
Embodiment 1
A kind of enzyme assisted extraction numb-taste components
(1) pretreatment of raw material: dry pericarpium zanthoxyli bungeani pericarp is crushed using pulverizer, and controlled 40 mesh of sieve.
(2) enzyme hydrolysis is handled: weighing in above-mentioned (1) Pricklyash peel by solid-liquid ratio 1:15 g/ml(w:v) addition distilled water,
And the complex enzyme of Pricklyash peel quality 2% is added (cellulase, hemicellulase and pectase proportions are 3:2:1);Using
Concussion is cultivated, and controls 40 DEG C of temperature, time 2.5h, pH4.5.
(3) spicy components are extracted: after above-mentioned (2) enzymatic treatment, pressing Pricklyash peel solid-liquid ratio 1:15g/ml(w immediately:
V) edible alcohol is added.Temperature 50 C, time 3h are controlled, is extracted using concussion mode.It is filtered, collects after to be extracted
Filtrate, and it is evaporated recycling edible alcohol, obtain numb-taste components crude extract.
(4) spicy components purify: spicy components primary extract in (3) is redissolved using edible alcohol, and in 4000r/min,
Solid impurity is removed under the conditions of 5min, collects supernatant;Then supernatant is passed through in macroporous adsorption resin chromatography column, collects fiber crops
Taste fraction;It is finally evaporated recycling edible alcohol, obtains numb-taste components.
Embodiment 2
A kind of enzyme assisted extraction numb-taste components
(1) pretreatment of raw material: dry pericarpium zanthoxyli bungeani pericarp is crushed using pulverizer, and controlled 40 mesh of sieve.
(2) enzyme hydrolysis is handled: weighing in above-mentioned (1) Pricklyash peel by solid-liquid ratio 1:15 g/ml(w:v) addition distilled water,
And the complex enzyme of Pricklyash peel quality 2% is added (cellulase, hemicellulase and pectase proportions are 2:1:1);Using
Concussion is cultivated, and controls 40 DEG C of temperature, time 2.5h, pH4.5.
(3) spicy components are extracted: after above-mentioned (2) enzymatic treatment, pressing Pricklyash peel solid-liquid ratio 1:15g/ml(w immediately:
V) edible alcohol is added.Temperature 50 C, time 3h are controlled, is extracted using concussion mode.It is filtered, collects after to be extracted
Filtrate, and it is evaporated recycling edible alcohol, obtain numb-taste components crude extract.
(4) spicy components purify: spicy components primary extract in (3) is redissolved using edible alcohol, and in 4000r/min,
Solid impurity is removed under the conditions of 5min, collects supernatant;Then supernatant is passed through in macroporous adsorption resin chromatography column, collects fiber crops
Taste fraction;It is finally evaporated recycling edible alcohol, obtains numb-taste components.
Embodiment 3
A kind of enzyme assisted extraction numb-taste components
(1) pretreatment of raw material: dry pericarpium zanthoxyli bungeani pericarp is crushed using pulverizer, and controlled 60 mesh of sieve.
(2) enzyme hydrolysis is handled: weighing in above-mentioned (1) Pricklyash peel by solid-liquid ratio 1:10 g/ml(w:v) addition distilled water,
And the complex enzyme of Pricklyash peel quality 2.5% is added (cellulase, hemicellulase and pectase proportions are 3:2:1);It adopts
It is cultivated with concussion, and controls temperature 45 C, time 3h, pH5.5.
(3) spicy components are extracted: after above-mentioned (2) enzymatic treatment, pressing Pricklyash peel solid-liquid ratio 1:10g/ml(w immediately:
V) edible alcohol is added.Temperature 60 C, time 3.5h are controlled, is extracted using concussion mode.It is filtered, receives after to be extracted
Collect filtrate, and be evaporated recycling edible alcohol, obtains numb-taste components crude extract.
(4) spicy components purify: spicy components primary extract in (3) is redissolved using edible alcohol, and in 5000r/min,
Solid impurity is removed under the conditions of 10min, collects supernatant;Then supernatant is passed through in macroporous adsorption resin chromatography column, is collected
Spicy components fraction;It is finally evaporated recycling edible alcohol, obtains numb-taste components.
Comparative example 1
A kind of edible alcohol extraction numb-taste components
Compared with Example 1, it is not added with complex enzyme.
(1) pretreatment of raw material: dry pericarpium zanthoxyli bungeani pericarp is crushed using pulverizer, and controlled 40 mesh of sieve.
(2) spicy components are extracted: pressing Pricklyash peel solid-liquid ratio 1:15g/ml(w:v) edible alcohol is added.Control temperature 50
DEG C, time 3h, extracted using concussion mode.It is filtered after to be extracted, collects filtrate, and be evaporated recycling edible alcohol,
Obtain numb-taste components crude extract.
(3) spicy components purify: spicy components primary extract in (2) is redissolved using edible alcohol, and in 4000r/min,
Solid impurity is removed under the conditions of 5min, collects supernatant;Then supernatant is passed through in macroporous adsorption resin chromatography column, collects fiber crops
Taste fraction;It is finally evaporated recycling edible alcohol, obtains numb-taste components.
Comparative example 2
A kind of enzyme assisted extraction numb-taste components
Compared with Example 1, Single Fiber element enzyme is only added.
(1) pretreatment of raw material: dry pericarpium zanthoxyli bungeani pericarp is crushed using pulverizer, and controlled 40 mesh of sieve.
(2) enzyme hydrolysis is handled: weighing in above-mentioned (1) Pricklyash peel by solid-liquid ratio 1:15 g/ml(w:v) addition distilled water,
And the cellulase of Pricklyash peel quality 2% is added;It is cultivated using concussion, and controls 40 DEG C of temperature, time 2.5h, pH4.5.
(3) spicy components are extracted: after above-mentioned (2) enzymatic treatment, pressing Pricklyash peel solid-liquid ratio 1:15g/ml(w immediately:
V) edible alcohol is added.Temperature 50 C, time 3h are controlled, is extracted using concussion mode.It is filtered, collects after to be extracted
Filtrate, and it is evaporated recycling edible alcohol, obtain numb-taste components crude extract.
(4) spicy components purify: spicy components primary extract in (3) is redissolved using edible alcohol, and in 4000r/min,
Solid impurity is removed under the conditions of 5min, collects supernatant;Then supernatant is passed through in macroporous adsorption resin chromatography column, collects fiber crops
Taste fraction;It is finally evaporated recycling edible alcohol, obtains numb-taste components.
Comparative example 3
A kind of enzyme assisted extraction numb-taste components
Compared with Example 1, cellulase, hemicellulase and pectase proportions are 1:1:1.
(1) pretreatment of raw material: dry pericarpium zanthoxyli bungeani pericarp is crushed using pulverizer, and controlled 40 mesh of sieve.
(2) enzyme hydrolysis is handled: weighing in above-mentioned (1) Pricklyash peel by solid-liquid ratio 1:15 g/ml(w:v) addition distilled water,
And the complex enzyme of Pricklyash peel quality 2% is added (cellulase, hemicellulase and pectase proportions are 1:1:1);Using
Concussion is cultivated, and controls 40 DEG C of temperature, time 2.5h, pH4.5.
(3) spicy components are extracted: after above-mentioned (2) enzymatic treatment, pressing Pricklyash peel solid-liquid ratio 1:15g/ml(w immediately:
V) edible alcohol is added.Temperature 50 C, time 3h are controlled, is extracted using concussion mode.It is filtered, collects after to be extracted
Filtrate, and it is evaporated recycling edible alcohol, obtain numb-taste components crude extract.
(4) spicy components purify: spicy components primary extract in (3) is redissolved using edible alcohol, and in 4000r/min,
Solid impurity is removed under the conditions of 5min, collects supernatant;Then supernatant is passed through in macroporous adsorption resin chromatography column, collects fiber crops
Taste fraction;It is finally evaporated recycling edible alcohol, obtains numb-taste components.
Test example
Test method and result (by taking pericarpium zanthoxyli bungeani as an example)
(1) 3 kind of complex enzyme ratio mixture experiment design result such as the following table 1:
1 cellulase of table, hemicellulose and pectase ratio mixture experiment design { 3,3 } result
。
Experimental design is carried out according to three factor of uniline grid, three rank grid point design principle in mixture experiment design, it is real to obtain table 1
It tests as a result, analyzed further according to mixture experiment design data software, obtains the relationship between respective function and actual constituent, finally ask
Optimal proportion numerical value is cellulase: hemicellulase out: pectase is 3:2:1 and 2:1:1.And two kinds of ratios are tested
Card, obtaining numb-taste components recovery rate is 11.5% and 11.4%, close with predicted value.Therefore, illustrate that the two ratios are true
It is credible, it can be used as optimum proportioning.
(2) embodiment is compared with comparative example result as shown in Fig. 1 and table 2:
The numb-taste components recovery rate comparison that 2 Different Extraction Method of table obtains
。
It is can be found that from Fig. 1 and 2 experimental result of table: in the embodiment 1-3 product extracted according to the method for the present invention, not only
Spicy components recovery rate is apparently higher than comparative example 1(compared with Example 1, is not added with complex enzyme), 2(compared with Example 1, only
Single Fiber element enzyme is added) and 3(is compared with Example 1, cellulase, hemicellulase and pectase proportions are 1:1:
1) it is more that the amide substance type that numb sense of taste is felt, and in the spicy components that extract is presented.Therefore, can obviously illustrate in this hair
The numb-taste components recovery rate prepared under the complex enzyme and its unique proportions of bright selection is higher, and amide in spicy components product
Substance type is more, and numb taste stimulation is stronger.
(3) electronic scanner microscope observes enzymatic treatment Chinese prickly ash eucaryotic cell structure
It will be evident that embodiment 1-3 Chinese prickly ash residue eucaryotic cell structure brokenization is serious from Fig. 2, there are a large amount of cavities.And comparative example
1(compared with Example 1, is not added with complex enzyme) in without addition enzymatic treatment, so occurring without obvious cavity.And comparative example 2
(Single Fiber element enzyme compared with Example 1, is only added) and comparative example 3(is compared with Example 1, cellulase, hemicellulase
After adding enzymatic treatment with pectase proportions for 1:1:1) is middle, there are a large amount of minuscule holes, but compared to embodiment 1-3, flower
Green pepper eucaryotic cell structure brokenization degree is slightly weak.Therefore, it can be said that bright, after the method for the present invention passes through enzymatic treatment, hence it is evident that broken to have changed Chinese prickly ash thin
Born of the same parents' structure is conducive to spicy components dissolution, increases recovery rate.
Claims (9)
1. a kind of method of enzyme assisted extraction numb-taste components, which is characterized in that this method comprises the following steps:
(1) pretreatment of raw material: dry Chinese prickly ash pericarp is crushed using pulverizer, sieve 40-60 mesh is crossed, it is standby to obtain Pricklyash peel
With;
(2) enzyme hydrolysis is handled: weighing Pricklyash peel by solid-liquid ratio 1:10-15(w:v) and distilled water is added, and Pricklyash peel matter is added
The enzyme of 2-2.5% is measured, control temperature, time, pH value carry out concussion cultivation, it is spare to obtain Pricklyash peel enzymolysis liquid;
(3) solvent extraction: by Pricklyash peel enzymolysis liquid press solid-liquid ratio 1:10-15(w:v) be added edible alcohol, control temperature, when
Between shake extract, filtered after to be extracted, collect filtrate, be evaporated recycling edible alcohol, it is standby to obtain numb-taste components crude extract
With;
(4) spicy components purify: redissolving numb-taste components crude extract using edible alcohol, and are centrifuged off solid impurity, receive
Collect supernatant, supernatant is passed through in macroporous adsorption resin chromatography column, collects spicy components fraction, be finally evaporated recycling edible wine
Essence obtains a kind of numb-taste components.
2. preparation method according to claim 1, which is characterized in that the Chinese prickly ash pericarp is selected from pericarpium zanthoxyli bungeani, rattan green pepper or blueness
One of Chinese prickly ash.
3. preparation method according to claim 1, which is characterized in that in the step (2) controlled at 40-45 DEG C,
The control time is 2.5-3h, control pH value is 4.5-5.5.
4. preparation method according to claim 1, which is characterized in that the enzyme is by cellulase, hemicellulase and fruit
Glue enzyme 3:2:1 in mass ratio composition.
5. preparation method according to claim 1, which is characterized in that the enzyme also by cellulase, hemicellulase and
Pectase 2:1:1 in mass ratio composition.
6. preparation method according to claim 1, which is characterized in that in the step (3) controlled at 50-60 DEG C,
The control time is 3-3.5h.
7. preparation method according to claim 1, which is characterized in that centrifugal condition is 4000- in the step (4)
5000r/min, centrifugation time 5-10min.
8. preparation method according to claim 3, which is characterized in that the regulation of the pH value is with the citric acid of 10mg/ml
It is adjusted.
9. numb-taste components made from a kind of any one method according to claim 1 ~ 8.
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