CN109349429A - A kind of soy sauce ketone extract and its application - Google Patents
A kind of soy sauce ketone extract and its application Download PDFInfo
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- CN109349429A CN109349429A CN201811483467.0A CN201811483467A CN109349429A CN 109349429 A CN109349429 A CN 109349429A CN 201811483467 A CN201811483467 A CN 201811483467A CN 109349429 A CN109349429 A CN 109349429A
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- soy sauce
- phagostimulant
- sauce ketone
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/10—Organic substances
- A23K20/116—Heterocyclic compounds
- A23K20/121—Heterocyclic compounds containing oxygen or sulfur as hetero atom
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- A—HUMAN NECESSITIES
- A23—FOODS OR FOODSTUFFS; TREATMENT THEREOF, NOT COVERED BY OTHER CLASSES
- A23K—FODDER
- A23K20/00—Accessory food factors for animal feeding-stuffs
- A23K20/20—Inorganic substances, e.g. oligoelements
- A23K20/28—Silicates, e.g. perlites, zeolites or bentonites
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- Polymers & Plastics (AREA)
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Abstract
The invention discloses a kind of soy sauce ketone extract and its preparing the application in phagostimulant, soy sauce ketone is opened in the new application of feed additive field, the present invention is based on soy sauce residues, soy sauce ketone extract is obtained by the methods of extracting, being concentrated, and press component: a kind of wholesome poultry phagostimulant is made in soy sauce ketone extract 20%~35%, zeolite powder 15%~25%, magnesium sulfate 15%~20%, potassium sulfate 20%~25%, sodium chloride 5%~15%, sodium bicarbonate 10~15%.Its beneficial effect is that the phagostimulant stable effective ingredients are low-consuming, easy to use, can dramatically increase poultry grazing rate；It has no toxic side effect, it is at low cost, it is environmentally protective, promote resource utilization；The preparation method is simple to operation, is suitable for large-scale promotion.
Description
Technical field
The invention belongs to field of feed additive technology, more particularly, to a kind of soy sauce ketone extract and its application.
Background technique
Soy sauce ketone (the entitled 2- methyl -5- ethyl -4- hydroxyl-furans -3- ketone of chemistry or 2- ethyl -5- methyl -4- hydroxyl -
Furans -3- ketone) also known as the high furanone of ring, nature be primarily present in soy sauce, therefore be called soy sauce ketone, be a kind of light yellow
Or yellow transparent liquid, there is high-intensitive sweet tea camerlsed, the natural fragrant and sweet and fruit aroma of paste flavor characteristic, while also having light
The fragrance of micro- baked goods.Soy sauce ketone flavor strength is 3~9 times of furanone, is to reconcile the important source material of essence and good
Fumet.It is now widely used in the food such as fruit, coffee, bread, maple syrup and beverage, tobacco, is that the U.S. eats producer
The safe edible fragrance that association (FEMA) is approved.Nearest Japanese scholars research discovery soy sauce ketone also has anti-tumor activity.
In livestock culture production, with the raising of productivity, the nutritional quality guaranteed in daily ration is not required nothing more than, is also required
Feed has good palatability and enough feed intakes, just can guarantee livestock and poultry to the aggregate demand of nutrient.Livestock and poultry are in stress situation
When, such as it is noisy, scaring, it is crowded, divide group, turn group, transport, wean, castration, sweltering heat, cold, will lead to appetite decrease, feeding
Amount decline.Phagostimulant is made of stimulation taste component and auxiliary agent, for improving feed palatability, promotes raising animal
Appetite, therefore, phagostimulant, which is added, in feed is very important.
Phagostimulant currently on the market is largely the combination of flavouring agent or sweetener or both, and function is more single, only
Can smell to animal or the sense of taste etc. form the constituent of single stimulation or even some flavouring agents or sweetener from change
Sintetics is learned, it is obvious easily to generate medicament residue, toxic side effect in animal body.It is common that there is fragrance, sweet taste (or appetite stimulating type
Composition) phagostimulant composition have: monosodium glutamate, saccharin, vomiting nut, betel nut, fennel, hawthorn, amino acid, molasses etc..
The soy sauce annual output of China's Mainland is in 5,000,000 t or so at present, and soy sauce market year increases 10% or more, and every life
1kg soy sauce is produced, about 0.67kg soy sauce residues will be generated.Soy sauce residues are the residues that moromi leaching oil pressure is squeezed or generated after pumping, and are in
Dark-brown.Main nutritional ingredient are as follows: crude fat content 7.4%~8.6%, crude protein 19.5%~25.8%, reduced sugar
10.7%~12.3%, crude fibre 48.3% or so.Since its yield is big, washiness, it is not easy to store and transports, if locating not in time
Comprehend smelly rotten quickly, causes the pollution of environment.If being directly used as feed easily causes animal poisoning, if for fertilizer or directly
Landfill will cause soil salinity characters.Soy sauce ketone is the main note substance of generation during soy sauce brewing, is the important natural activity of soy sauce
Substance.
Summary of the invention
The invention discloses a kind of soy sauce ketone extract and its application in phagostimulant is being prepared, soy sauce ketone is being opened and is raising
The new application in feed additives field, while soy sauce residues comprehensive utilization of resources is improved using soy sauce residues as raw material to extract soy sauce ketone
Rate also avoids it and pollutes the environment.
The specific technical solution of the present invention is as follows:
The present invention provides a kind of soy sauce ketone extract, the soy sauce ketone extract be by soy sauce residues through solvent extraction and
, wherein solvent is water or 15~40% ethanol solutions.
Further, the solvent is 20% ethanol solution.
Further, the soy sauce ketone extract the preparation method comprises the following steps: weigh soy sauce residues, added by solid-liquid ratio 1: 8~10 molten
5~10h is impregnated in agent after mixing evenly, and 5~10min is centrifuged under 1000~5000rpm revolving speed, then takes supernatant concentration dry
It is dry to obtain soy sauce ketone extract, wherein the temperature being concentrated and dried is 40~60 DEG C.
Further, content of the soy sauce ketone in soy sauce ketone extract is 50~500ppm.Soy sauce ketone are as follows: 5- ethyl -4- hydroxyl
- 3 (2H)-furanone of base -2- methyl, -3 (2H)-furanone of 2- ethyl -4- hydroxy-5-methyl base or above two compound it is same
Enantiomers, the above substance and its content have a significant impact to attractant effect of the invention is played.
Further, the soy sauce ketone extract soy sauce ketone is preparing the application in phagostimulant, the food calling pair of the phagostimulant
As for chicken or pig.
Further, the phagostimulant is according to mass percent, including following component:
Soy sauce ketone extract 20%~35%, 100 mesh~200 mesh zeolite powder 15%~25%, magnesium sulfate 15%~
20%, potassium sulfate 20%~25%, sodium chloride 5%~15%, sodium bicarbonate 10~15%.
Further, the preparation of the phagostimulant includes the following steps:
S1: measuring water, is separately added into magnesium sulfate, potassium sulfate and sodium chloride and mixed solution is made；Magnesium sulfate and potassium sulfate are
In order to form the microelement crystallization of uniform, useful space structure, there is slow releasing function, sodium chloride is primarily to provide salty wind
Taste, in addition chloride ion participates in the generation of gastric acid in vivo, and also has effect in the normal excitability for maintaining nerves and muscles；
S2: it will be mixed after soy sauce ketone extract addition zeolite powder with mixed solution in step S1, to guarantee that product is uniform, steady
Surely it need to be placed in high pressure homogenizer, pressure is 3~10Mpa, homogeneous 2~5 times, every time 5~10min, then be spray-dried, obtain drying
Object, wherein the good smell that can be effectively retained paste flavor is used in combination in the features such as zeolite powder surface porosity is porous, uniform adsorption,
Other microelements are adsorbed simultaneously, it, can slow release active principle in animal body during digestion and metabolism；
S3: sodium bicarbonate is added in step S2 in dried object and is uniformly mixed, phagostimulant is obtained.Wherein, sodium bicarbonate
Play buffering.
Further, 120~200 DEG C of the intake air temperature of spray drying described in the step S2, air outlet temperature 60~
100℃。
Further, the mass percent that the phagostimulant adds in feed is 0.3%~0.6%.
The present invention also provides a kind of soy sauce ketone to prepare the application in phagostimulant, the soy sauce ketone are as follows: 5- ethyl -4- hydroxyl
- 3 (2H)-furanone of base -2- methyl, -3 (2H)-furanone of 2- ethyl -4- hydroxy-5-methyl base or above two compound it is same
One of enantiomers are a variety of；The food calling object of the phagostimulant is chicken or pig.
The present invention sufficiently develops and uses soy sauce residues resource, and one kind is made using other compound active principles of soy sauce ketone extract
Poultry phagostimulant can dramatically increase feed palatability, improve poultry grazing rate, while improving resource utilization, solve soy sauce residues
The harm problem that environment is generated.
Compared with the existing technology, the present invention has the advantage that and effect:
1. the phagostimulant stable effective ingredients, low-consuming, easy to use, poultry grazing rate can be dramatically increased.
2. this method is simple to operation, it is suitable for large-scale promotion.
3. it has no toxic side effect, it is at low cost, it is environmentally protective, promote resource utilization.
Detailed description of the invention
Fig. 1 is that soy sauce ketone standard items GC-MS analyzes total ion current figure.
Fig. 2 is the corresponding MS map in No. 1 peak.
Fig. 3 is the corresponding MS map in No. 2 peaks.
Fig. 4 is that soy sauce ketone (sample sets) analyzes GC-MS total ion current figure in soy sauce residues.
Fig. 5 is that sample sets+standard items analyze GC-MS total ion current figure.
Specific embodiment
Further illustrate the present invention below in conjunction with specific embodiment, but embodiment the present invention is not done it is any type of
It limits.Unless stated otherwise, the present invention uses reagent, method and apparatus is the art conventional reagents, method and apparatus.
Unless stated otherwise, agents useful for same and material of the present invention are commercially available.
Soy sauce residues purchase is in soy sauce factory, main nutritional ingredient are as follows: crude fat content in following embodiment and experimental example
7.4%~8.6%, crude protein 19.5%~25.8%, reduced sugar 10.7%~12.3%, crude fibre 45.0~49.3%.
Embodiment 1
A kind of phagostimulant and preparation method thereof that soy sauce ketone extract compounds, includes the following steps:
S1: the preparation of soy sauce ketone extract:
Soy sauce residues 1kg is weighed, 40% ethanol solution is added by solid-liquid ratio 1: 10, impregnates 10h, 1000rpm after mixing evenly
It is centrifuged 5min under revolving speed, supernatant is taken to be concentrated to give soy sauce ketone extract, measuring soy sauce ketone content is 120ppm, wherein the temperature being concentrated
Degree is 40 DEG C；
S2: measuring 1000mL water, is separately added into magnesium sulfate 200g, potassium sulfate 200g and the obtained mixing of sodium chloride 100g is molten
Liquid；
S3: it by soy sauce ketone extract 240g in step S1, adds and presses 1: 1 with mixed solution in step S2 after 160g zeolite powder
Mixing, stirs evenly and is placed in high pressure homogenizer, pressure 5Mpa, and homogeneous 3 times, each 5min, then in intake air temperature 180
DEG C, it is dry under 90 DEG C of spray drying conditions of air outlet temperature, obtain dried object；
S4: sodium bicarbonate 100g is added in step S3 in dried object and is uniformly mixed, phagostimulant is obtained.
Embodiment 2
A kind of phagostimulant and preparation method thereof that soy sauce ketone extract compounds, includes the following steps:
S1: the preparation of soy sauce ketone extract:
Soy sauce residues 1kg is weighed, adds 20% ethanol solution by solid-liquid ratio 1: 8, impregnates 5h after mixing evenly, 2000rpm turns
Speed is lower to be centrifuged 5min, takes supernatant to be concentrated to give soy sauce ketone extract, measuring soy sauce ketone content is 224ppm, wherein the temperature being concentrated
It is 40 DEG C；
S2: measuring 1000mL water, is separately added into magnesium sulfate 180g, potassium sulfate 220g and mixed solution is made in sodium chloride 80g；
S3: it by soy sauce ketone extract 220g in step S1, adds and presses 1: 1 with mixed solution in step S2 after 180g zeolite powder
Mixing, stirs evenly and is placed in high pressure homogenizer, pressure 5Mpa, and homogeneous 3 times, each 5min, then in intake air temperature 180
DEG C, it is dry under 90 DEG C of spray drying conditions of air outlet temperature, obtain dried object；
S4: sodium bicarbonate 120g is added in step S3 in dried object and is uniformly mixed, phagostimulant is obtained.
Experimental example one
The research of soy sauce ketone crude extract extraction conditions
After extracting 3 times with different solvents (by solid-liquid ratio 1: 10) to soy sauce residues, merges 3 extracting solutions, then take
Equal amount carries out direct sense organ Olfactive evaluation after natural solvent flashing in glass culture dish:
The subjective appreciation of the soy sauce ketone runic object of the different extracting modes of table 1
The result shows that: it is more with pure water, 20% ethyl alcohol, the taste compound of 40% ethanol extract, judge by sense organ,
It is most dense that 20% ethyl alcohol extracts paste flavor substance taste.
Experimental example two
Soy sauce ketone constituent analysis in soy sauce residues --- GC-MS analysis detection
(1) soy sauce ketone standard items configure: soy sauce ketone reference substance, and purity is 98% (Fu Bang International Holdings Ltd)
1. the soy sauce ketone reference substance for taking 90mg embodiment 2 to obtain crosses 0.22 with 10mL is settled in anhydrous ether after shaking up
μm filter membrane, takes final proof to be analyzed with GC-MS；
2. taking 90mg soy sauce ketone extract sample, with 10mL is settled in dehydrated alcohol, 0.22 μm of filter membrane is crossed after shaking up, is taken
Upper final proof is analyzed with GC-MS；
(2) the GC-MS analysis detection of soy sauce ketone
GC condition: chromatographic column is DB-5MS quartz capillary column (30m × 0.25mm, 0.25 μm)；Preceding injector temperature 250
℃；Flow rate of carrier gas: 1.0mL/min (high-purity helium)；Split ratio is 50: 1；Temperature program: 40 DEG C of operation 1min；Then 10 DEG C/
Min to 120 DEG C of operation 5min；Then 15 DEG C/min to 250 DEG C of operation 5min (runing time 27.67min in total).
The end MS parameter: accessory channel temperature: 280 DEG C, 150 DEG C of level four bars temperature, ion source temperature: 230 DEG C；Acquisition side
Formula: full scan；Scanning quality range: 40~330aum；Sample volume: 1 μ L.Qualitative, peak area progress is carried out using appearance time
It is quantitative.
(3) soy sauce ketone standard items GC-MS is analyzed
If Fig. 1 is soy sauce ketone standard items GC-MS analysis chromatogram, pass through the isomer with report soy sauce ketone in document
Mass spectrogram 2 and Fig. 3 comparison, so that it is determined that: No. 1 peak corresponds to -3 (2H)-furanone of 5- ethyl -4- hydroxy-2-methyl；No. 2 peaks pair
Answer -3 (2H)-furanone of 2- ethyl -4- hydroxy-5-methyl base.
There are the soy sauce ketone of two kinds of forms (- 3 (2H)-furanones of 5- ethyl -4- hydroxy-2-methyl in soy sauce residues；2- second
- 3 (2H)-furanone of base -4- hydroxy-5-methyl base), total content 242.25ppm.
(4) sample detection result
Pass through (mark encloses) time (see Fig. 4) of appearance in contrast sample and standard items and the GC-MS map of sample mark-on group
(see Fig. 5), it can be clearly seen that containing there are two types of the soy sauce ketone (5- ethyl -4- hydroxy-2-methyls -3 (2H)-of configuration in soy sauce residues
Furanone；- 3 (2H)-furanone of 2- ethyl -4- hydroxy-5-methyl base).Then quantitative analysis is carried out by peak area, be calculated
Two kinds of soy sauce ketone isomers are coexisted with 1: 2 ratio, and be consistent (Monde K et al., 2009) with document report, and total content is
242.25ppm。
Experimental example three
Phagostimulant effect experiment
Choose that 20 weight are close, the good piglet of body condition, average weight is 15.5 kilograms, is divided into 2 groups, feeds base respectively
The test creep feed (experimental group) of plinth creep feed (control group) and addition addition soy sauce ketone phagostimulant.Experimental period 10 days.Each reality
It tests and is repeated 3 times.
2 phagostimulant effect experiment of table
The result shows that being averaged for weanling pig can be significantly improved by adding soy sauce ketone phagostimulant compared with the control group, in child care material
Daily ingestion amount (6.342kg vs 5.578kg, P < 0.05).Comprehensive analysis, soy sauce ketone phagostimulant is in groove feed for pigling and child care
The growth performance of piglet can be improved in fit applications in material.
Embodiment described above, only two kinds of more preferably concrete modes of the present invention, those skilled in the art are in this hair
The usual variations and alternatives carried out in bright technical proposal scope should all be included in protection scope of the present invention.
Claims (10)
1. a kind of soy sauce ketone extract, which is characterized in that the soy sauce ketone extract is to obtain soy sauce residues through solvent extraction,
In, solvent is water or 15~40% ethanol solutions.
2. soy sauce ketone extract according to claim 1, which is characterized in that the solvent is 20% ethanol solution.
3. soy sauce ketone extract according to claim 2, which is characterized in that the preparation method of the soy sauce ketone extract
Are as follows: soy sauce residues are weighed, solvent is added by solid-liquid ratio 1: 8~10, impregnates 5~10h after mixing evenly, are turned in 1000~5000rpm
Speed is lower to be centrifuged 5~10min, and supernatant is then taken to be concentrated and dried to obtain soy sauce ketone extract, wherein the temperature being concentrated and dried be 40~
60℃。
4. soy sauce ketone extract as claimed in any of claims 1 to 3, which is characterized in that soy sauce ketone is in soy sauce ketone
Content in extract is 50~500ppm.
5. soy sauce ketone extract described in a kind of any one of Claims 1-4 exists preparing the application in phagostimulant, feature
In the food calling object of the phagostimulant is chicken or pig.
6. soy sauce ketone extract is preparing the application in phagostimulant according to claim 5, which is characterized in that the phagostimulant
According to mass percent, including following component:
Soy sauce ketone extract 20%~35%, 100 mesh~200 mesh zeolite powder 15%~25%, magnesium sulfate 15%~20%, sulphur
Sour potassium 20%~25%, sodium chloride 5%~15%, sodium bicarbonate 10~15%.
7. soy sauce ketone extract is preparing the application in phagostimulant according to claim 6, which is characterized in that the phagostimulant
Preparation include the following steps:
S1: measuring water, is separately added into magnesium sulfate, potassium sulfate and sodium chloride and mixed solution is made；
S2: mixing after soy sauce ketone extract is added zeolite powder with mixed solution in step S1, stirs evenly that be placed on high pressure equal
In matter machine, pressure is 3~10Mpa, homogeneous 2~5 times, every time 5~10min, then be spray-dried, obtain dried object；
S3: sodium bicarbonate is added in step S2 in dried object and is uniformly mixed, phagostimulant is obtained.
8. soy sauce ketone extract is preparing the application in phagostimulant according to claim 7, which is characterized in that the step S2
Described in 120~200 DEG C of the intake air temperature of spray drying, 60~100 DEG C of air outlet temperature.
9. soy sauce ketone extract described according to claim 6 or 7 is preparing the application in phagostimulant, which is characterized in that described to lure
The mass percent that food agent is added in feed is 0.3%~0.6%.
10. soy sauce ketone is preparing the application in phagostimulant, which is characterized in that the soy sauce ketone are as follows: 5- ethyl -4- hydroxyl -2- first
The isomer of base -3 (2H)-furanone, -3 (2H)-furanone of 2- ethyl -4- hydroxy-5-methyl base or above two compound
One of or it is a variety of；The food calling object of the phagostimulant is chicken or pig.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111459117A (en) * | 2020-04-28 | 2020-07-28 | 四川合江县永兴诚酿造有限责任公司 | Soy sauce ancient method brewing full-flow monitoring system |
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Application publication date: 20190219 |