CN102657326B - Natural lentmus edodes powder and extracting method and application thereof - Google Patents
Natural lentmus edodes powder and extracting method and application thereof Download PDFInfo
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Abstract
The invention discloses natural lentmus edodes powder and an extracting method and application thereof. The extracting method comprises the steps of adding dried lentmus edodes (lentmus edodes sing.) powder into water, performing steam distillation and extraction for 1-4hours, and collecting distillate to obtain natural lentmus edodes powder, wherein the water is supplemented in a mixture of the dried lentmus edodes powder and the water in the process of the steam distillation and extraction. The extracting method is simple in process, short in reaction time, low in energy consumption and low in cost, the extracting yield rate of 1,2,3,5,6-penta-sulphur cycloheptane is high, and additional value and comprehensive utilization ratio of the lentmus edodes are effectively improved. The natural lentmus edodes powder prepared by the extracting method contains more than thirty types of flavor substance, is high in sulfocompound relative content, rich in ingredients, rich in flavor, realistic in fragrance and free of organic solvent, reaches food security level, can be directly prepared into seasoning to be added into a product for flavor blending and is especially suitable for preparing house-hold delicate-flavor seasonings, fungus sauces or seasonings of canned mushrooms and convenience foods.
Description
Technical field
The present invention relates to essence and flavoring agent field, relate in particular to a kind of natural mushroom essence and extracting method and application.
Background technology
Mushroom (Lentinus edodes Sing.) is a kind of edible mushroom having long enjoyed a good reputation in China, with the local flavor of its abundant nutrition, uniqueness, is deeply subject to liking of broad masses.Meanwhile, mushroom is also a kind of medicinal fungi, and research in recent years shows, it contains the plurality of active ingredients such as lentinan, eritadenine, vitamin and adenosine, has the body immunity of raising, antitumor, hypoglycemic, reducing blood lipid and the effect such as antiviral.
The peculiar flavour of mushroom is its wide ace-high one large major reason, becomes the focus of Recent study about its detection analysis of volatile ingredient.Research shows, C8 compound, as 1-OCOL, 2-octen-1-ol; Sulfur-containing compound, comprises 1,2,4-trithio pentamethylene, 1,2,4, and 5-tetra-sulphur cyclohexanes and 1,2,3,5,6-, five sulphur cycloheptane etc. are mushroom main volatile chemical composition, are closely related with its characteristic flavor on basis.In China, in order to be beneficial to preservation, mushroom is resaled after being often prepared to dried thin mushroom, is eaten, and the generation of the peculiar flavour of mushroom pleasant also process drying with it is closely related.
Mushroom essence (Lenthionine) refers to 1,2,3,5,6-, five sulphur cycloheptane in chemical sense, but can be also the general name of volatile flavor substance in dried thin mushroom.1,2,3,5,6-, five sulphur cycloheptane are that a kind of molecular formula is the volatile cyclic sulfur-containing compound of C2H4S5, are considered to the key odorant composition of dried thin mushroom, its fragrance is strong, and characteristic is strong, is used as at present main component and is widely used in mushroom flavour product and lenthionine.But current as 1,2,3,5 of product sale, 6-five sulphur cycloheptane are mainly prepared by chemical synthesis process, its fragrance is single, the fragrant punching of head, but a little less than body note, whole fragrance is thiner.And the method condition harsh (low temperature-78 ℃) of synthetic 1,2,3,5,6-, the five sulphur cycloheptane of tradition, operating process need be through repeatedly extraction, separation, and the reaction time is long, and yield is low.
The people such as Yang Kai be take mushroom as raw material, adopt extraction by steam distillation mushroom essence, be specially: first determined mushroom steam distillation gained general volatile material---the ratio analysis method of mushroom essence, then by a plurality of single factor experiments, determine that the Optimized Extraction Process condition of mushroom essence steam distillation is: 50g raw meal is broken to 100 orders, by 1: 15 solid-to-liquid ratio, add in 2L round-bottomed flask, steam distillation is extracted 2h.Again in conjunction with gas chromatograph-mass spectrometer analysis, composition during mushroom rectifying under Optimizing Technical is divided is analyzed, detect and comprise that (poplar opens for 13 kinds of compounds of main taste compound, Sun Peilong, Zheng builds forever etc. a kind of extraction of mushroom essence and constituent analysis, China's flavouring, 2005,6: 24-28.).The method can be extracted and obtain mushroom essence from mushroom, but the spectrophotometric detecting method accuracy that it adopts is not high, can not reflect quantitatively each composition of mushroom essence particularly 1,2,3, the yield of 5,6-, five sulphur cycloheptane, therefore might not obtain the high product of mushroom essence yield according to its Optimizing Technical; Meanwhile, only detect 13 kinds of compounds in the product that the method makes, composition is less, may extract operating process flavor composition and lose larger.And the quantitative determination of the preparation of natural mushroom essence and yield thereof is had no to document announcement at present.
Summary of the invention
The invention provides a kind of extracting method of natural mushroom essence, for high yield prepare the mushroom essence that many, the natural safety of flavor components, fragrance are true to nature.
An extracting method for natural mushroom essence, comprising: mushroom (Lentinus edodes Sing.) dry powder is added to the water, and steam distillation is extracted 1-4h, collects distillate, obtains natural mushroom essence;
Wherein, in steam distillation leaching process, in the mixture (being mushroom feed liquid) of mushroom dry powder and water, add water.
Described mushroom kind is the large mushroom of light face, the little mushroom of light face, Qingyuan 241 or Qingyuan 9015; Be preferably the large mushroom of light face.Different its flavor substances of mushroom kind are micro-variant, but general characteristic local flavor is similar, are all that the sulfur-containing compound that is representative with 1,2,3,5,6-sulphur cycloheptane is as the main contributions composition of its characteristic flavor on basis.
Described mushroom dry powder obtains by mushroom drying, after pulverizing; Preferably, described mushroom dry powder obtains by the cap drying of mushroom, after pulverizing, and mushroom cap water content is at 8-12%.The contained flavor substance kind of mushroom cap and bacterium bar, content is difference to some extent all, mushroom local flavor is played to the sulfur-containing compound of main contributions effect and C8 compound etc. and mainly concentrate on cap part, bacterium bar than cap more linear paraffins and phenyl ring, heterocyclic compound, this may be with bacterium bar containing more cellulose, thereby and suberization occurs causes its flavor components difference relevant.
The particle diameter of described mushroom dry powder is 60-100 order; Be preferably 60-80 order; 60 orders more preferably.The object of pulverizing is to increase the contact area between feed liquid, and therefore sample is pulverized more carefully better in theory, and therefore, when mushroom dry powder particle diameter is between 60-100 order, natural mushroom essence yield is all higher.But it is meticulous that sample is pulverized, can affect solvent the flowing of storeroom, and can make the viscosity suction-operated on volatile ingredient and sample particle surface strengthen, affected overflowing of volatile ingredient, therefore,, when mushroom dry powder particle diameter is 60 order, the yield of natural mushroom essence is higher.
When mushroom dry powder is added to the water, described mushroom dry powder and the weight ratio of water are 1: 10-1: 12; Be preferably 1: 10.Increase the water yield, during heating, the water required heat that seethes with excitement also increases, thereby causes the steam of evaporation in same time to reduce, and the mushroom essence total amount of being carried secretly by it also reduces.The weight ratio of mushroom dry powder and water is 1: 10 o'clock, and the extraction yield of natural mushroom essence is the highest.
The vapo(u)rizing temperature of described steam distillation is 95-99 ℃.Vapo(u)rizing temperature is too low, is unfavorable for that water carries volatile materials to steam secretly; And vapo(u)rizing temperature is too high, part volatile materials can be hydrolyzed, oxidation, esterification or thermal decomposition, and even decomposing the little molecule obtaining can cross reaction generate the material that affects local flavor.After mushroom dry powder mixes with water, boiling point declines, and the boiling point (100 ℃) lower than pure water, adopts the vapo(u)rizing temperature of 95-99 ℃, can make mushroom feed liquid keep boiling, can reduce again the loss of volatile materials, saves energy consumption simultaneously.
The extraction time of described steam distillation is preferably 1.5-2.5h; 2-2.5h more preferably.In certain limit, extend extraction time and be conducive to steaming of volatile flavor substance; But overlong time is unfavorable for saving the needs of the energy, and along with the prolongation of heat time, can generates some and destroy the natural flavour mountaineous new component of mushrooms, the overall quality of product is exerted an influence.
The condensation of described steam distillation adopts the three step condensation methods that comprise air setting, 8-13 ℃ water condensation, 4-10 ℃ water condensation.The mode that three step condensation methods reduce step by step with temperature is carried out condensation to distillate, and the cooling flavor substance evaporating, reduces their volatilization loss more quickly, and makes the flavor substance that obtains more complete, presses close to the local flavor of natural mushroom.
The device of described steam distillation can adopt synchronous distilling and extracting device (SDE), and synchronous distilling and extracting device is reproducible, recovery rate is high, can realize the three step condensations to distillate, is particularly suitable for the extraction of volatile materials.In order to obtain directly available natural mushroom essence, do not use the organic matter extraction part in synchronous distilling and extracting device, and only use its steam distillation part.
When steam distillation is extracted, moisture steams gradually, is collected with the single-minded same condensation of mushroom, causes the water in mushroom feed liquid to reduce gradually, affects the extraction efficiency of mushroom essence; In mushroom feed liquid, add in time, continuously water, sufficient moisture can be provided, thereby the extraction efficiency that maintains mushroom essence is in higher level.
Preferably, the described speed of adding water during with steam distillation distillate to distillate speed identical, can make like this mushroom feed liquid keep suitable solid-liquid ratio always, guarantee fully steaming of volatile flavor substance.
Preferably, adopting the water replanishing device being connected with steam distillation device is that mushroom feed liquid is added water, add the speed of water and control by being arranged on the flow control valve on tube connector between steam distillation device and water replanishing device, and precise control, easy to operate.
In order to obtain the natural mushroom essence that concentration is higher, can carry out centrifugal treating to collecting the distillate obtaining, after finishing dealing with, get precipitum, obtain described natural mushroom essence.Adopt centrifugal treating, can farthest reduce the volatilization of flavor components.
The extracting method of above-mentioned natural mushroom essence can be carried out at mushroom comprehensive processing and utilization pretreatment stage, as while extracting functional components lentinan in mushroom, eritadenine, mushroom peptide etc., all can carry out water heating lixiviate of the present invention to mushroom sample early stage processes, in this processing procedure, collect the Flavor Compounds in Lentinus edodes because of heating volatilization, obtain natural mushroom essence, can greatly improve added value and the comprehensive utilization ratio of mushroom.
The invention provides a kind of natural mushroom essence that adopts said extracted method to obtain.This natural mushroom essence is the turbid shape liquid of milky,, containing any organic solvent, is not aliment security level.Evidence, take dried thin mushroom cap as the natural mushroom essence that raw material makes, and wherein contains more than 30 kind of flavor substance, comprises more than ten kind of sulfur-containing compound (relative amount reaches 23% left and right), and fragrance is abundant, with rich flavor, approaches dried thin mushroom fragrance.
The present invention also provides the application of above-mentioned natural mushroom essence in preparing mushroom flavour product.This natural mushroom essence is water extract, and containing organic solvent, security is not good, can directly or make and add to after condiment in product or food for blending, is particularly useful for making homely delicate flavour condiment, mushroom sauce, or the blending of canned mushroom, instant food.
The present invention be take dried thin mushroom as raw material, adopts steam distillation and moisturizing operation to match, and by suitable technological process and technological parameter, extracts and has obtained natural mushroom essence.
Adopt the inventive method, there is following beneficial effect:
(1) compare the features such as traditional chemical method is synthesized 1,2,3,5,6-, five sulphur cycloheptane, and it is simple that the inventive method has technique, and the reaction time is short, and energy consumption is low, and cost is low.
(2) adopt the inventive method, natural mushroom essence extraction efficiency is high, particularly 1,2,3,5,6-five sulphur cycloheptane, its yield can reach 13.5 μ g/g (with mushroom dry weight basis), is that at present known unique mushroom essence of appearing in the newspapers quantizes yield, and is significantly higher than conventional steam distillation extraction (general volatile flavor substance yield is 6.2 μ l/g only).
(3) extract the natural mushroom essence obtain and contain more than 30 kind of flavor substance, its sulfur-containing compound relative amount is high especially, with traditional chemical synthetic 1,2,3,5,6-five sulphur cycloheptane are compared, composition is abundant, with rich flavor, fragrance is true to nature; For water extract, containing organic solvent, be aliment security level, can directly or make and add to after condiment in product for blending, be particularly useful for making homely delicate flavour condiment, mushroom sauce, or the blending of canned mushroom, instant food.Prepared mushroom flavour product is safer, and fragrance is more true to nature, has boundless market prospects.
(4) the inventive method can be implemented at the pretreatment stage of mushroom comprehensive utilization process, in functional components such as extracting lentinan, eritadenine, champignon polypeptide, in earlier stage carry out flooding of the present invention, can synchronous collection the Flavor Compounds in Lentinus edodes of volatilization, greatly improved added value and the comprehensive utilization ratio of mushroom.
Accompanying drawing explanation
Fig. 1 is that the embodiment of the present invention 1 be take the mushroom essence that dried thin mushroom cap obtains as raw material extracts and detected and analyze the volatile ingredient TIC obtaining through GC-MS.
Fig. 2 is that the embodiment of the present invention 2 be take the mushroom essence that dried thin mushroom bacterium bar obtains as raw material extracts and detected and analyze the volatile ingredient TIC obtaining through GC-MS.
The specific embodiment
The extraction of the natural mushroom essence of embodiment 1
(1) get the cap of dried thin mushroom (kind is the large mushroom of light face), pulverize and sieve, obtain 60 order powder samples, be mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder is placed in 2000ml, add the distilled water of 10 times of weight ratios, mix, obtain mushroom feed liquid.
(3) on there-necked flask, install agitator, synchronous distilling and extracting device (SDE) and water replanishing device;
Wherein, water replanishing device is a leveling bottle, and the water outlet in body side is connected with rubber tube, and rubber tube inserts in there-necked flask after connecting glass tube; Flow control valve is housed on rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 2h, control vapo(u)rizing temperature at 99 ℃, keep the boiling of mushroom feed liquid.In still-process, mushroom essence is entered condenser pipe (comprising successively air set pipe, 8 ℃ of water condensing tubes, 4 ℃ of water condensing tubes) by the folded band of steam, cooled mushroom essence is mixed the turbid shape liquid that is creamy white with water, enter in the U-shaped pipe of condenser pipe lower end, by U-shaped pipe lower part outlet, can collect and obtain the aqueous natural mushroom essence of milkiness.
Wherein, when mushroom liquor boiling, steam starts, after condensation, to open flow control valve, and the water in water replanishing device is added in mushroom feed liquid; In whole leaching process, adjust flux control valve, controls and to add water speed and distillate to distillate speed consistent.
Take dipropyl disulfide as internal standard compound, set up the gas-chromatography detection method of mushroom essence content, each component content in the natural mushroom essence that Detection and Extraction obtain, obtains wherein 1,2,3,5, and the yield of 6-five sulphur cycloheptane is 13.5 μ g/g (with mushroom dry weight basis).
Adopt the analysis of GC-MS method to extract in the natural mushroom essence obtaining to become to be grouped into, draw: volatile ingredient identifies 36 kinds altogether, wherein sulfur-containing compound has 10 kinds, and relative amount reaches 23.648% volatile ingredient TIC and sees Fig. 1.
Composition in the natural mushroom essence of table 1 (take dried thin mushroom cap as raw material)
The extraction of the natural mushroom essence of embodiment 2
(1) get the bacterium bar of dried thin mushroom (kind is the large mushroom of light face), pulverize and sieve, obtain 60 order powder samples, be mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder is placed in 2000ml, add the distilled water of 10 times of weight ratios, mix, obtain mushroom feed liquid.
(3) on there-necked flask, install agitator, synchronous distilling and extracting device (SDE) and water replanishing device;
Wherein, water replanishing device is a leveling bottle, and the water outlet in body side is connected with rubber tube, and rubber tube inserts in there-necked flask after connecting glass tube; Flow control valve is housed on rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 2h, control vapo(u)rizing temperature at 99 ℃, keep the boiling of mushroom feed liquid.In still-process, mushroom essence is entered condenser pipe (comprising successively air set pipe, 8 ℃ of water condensing tubes, 4 ℃ of water condensing tubes) by the folded band of steam, cooled mushroom essence is mixed the turbid shape liquid that is creamy white with water, enter in the U-shaped pipe of condenser pipe lower end, by U-shaped pipe lower part outlet, can collect and obtain the aqueous natural mushroom essence of milkiness.
Wherein, when mushroom liquor boiling, steam starts, after condensation, to open flow control valve, and the water in water replanishing device is added in mushroom feed liquid; In whole leaching process, adjust flux control valve, controls and to add water speed and distillate to distillate speed consistent.
Adopt the analysis of GC-MS method to extract in the natural mushroom essence obtaining to become to be grouped into, draw: volatile ingredient identifies 63 kinds altogether, wherein sulfur-containing compound has 11 kinds, although relative amount 3.381% visible in sulfur-containing compound kind mushroom bacterium bar and cap difference little, but difference is more obvious on relative sulfur-bearing, sulfur-containing compound is the main contributions composition of dried thin mushroom flavour, in mushroom bacterium bar, all kinds volatile ingredient is more, comprise some linear paraffins and phenyl ring, heterocyclic compound, this may be with bacterium bar containing more cellulose, and possible suberization and cause its flavor components difference relevant.The content of sulfur-containing compound is not preponderated, thereby the flavour of dried thin mushroom bacterium bar is outstanding not as good as cap, shows to choose mushroom cap and has more advantage as the raw material that extracts mushroom essence.Mushroom bacterium bar volatile ingredient TIC is shown in Fig. 2.
Composition in the natural mushroom essence of table 2 (the dried thin mushroom bacterium bar of take is raw material)
The extraction of the natural mushroom essence of embodiment 3
(1) get the cap of dried thin mushroom (kind is Qingyuan 241), pulverize and sieve, obtain 80 order powder samples, be mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder is placed in 2000ml, add the distilled water of 10 times of weight ratios, mix, obtain mushroom feed liquid.
(3) on there-necked flask, install agitator, synchronous distilling and extracting device (SDE) and water replanishing device;
Wherein, water replanishing device is a leveling bottle, and the water outlet in body side is connected with rubber tube, and rubber tube inserts in there-necked flask after connecting glass tube; Flow control valve is housed on rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 2.5h, control vapo(u)rizing temperature at 97 ℃, keep the boiling of mushroom feed liquid.In still-process, mushroom essence is entered condenser pipe (comprising successively air set pipe, 10 ℃ of water condensing tubes, 6 ℃ of water condensing tubes) by the folded band of steam, cooled mushroom essence is mixed the turbid shape liquid that is creamy white with water, enter in the U-shaped pipe of condenser pipe lower end, by U-shaped pipe lower part outlet, can collect and obtain the aqueous natural mushroom essence of milkiness.
Wherein, when mushroom liquor boiling, steam starts, after condensation, to open flow control valve, and the water in water replanishing device is added in mushroom feed liquid; In whole leaching process, adjust flux control valve, controls and to add water speed and distillate to distillate speed consistent.
Adopt each component content in the natural mushroom essence that gas chromatography Detection and Extraction obtain, obtain wherein 1,2,3,5, the yield of 6-five sulphur cycloheptane is 13.0 μ g/g (with mushroom dry weight basis).
The extraction of the natural mushroom essence of embodiment 4
(1) get the cap of dried thin mushroom (kind is the little mushroom of light face), pulverize and sieve, obtain 100 order powder samples, be mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder is placed in 2000ml, add the distilled water of 12 times of weight ratios, mix, obtain mushroom feed liquid.
(3) on there-necked flask, install agitator, synchronous distilling and extracting device (SDE) and water replanishing device;
Wherein, water replanishing device is a leveling bottle, and the water outlet in body side is connected with rubber tube, and rubber tube inserts in there-necked flask after connecting glass tube; Flow control valve is housed on rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 1.5h, control vapo(u)rizing temperature at 99 ℃, keep the boiling of mushroom feed liquid.In still-process, mushroom essence is entered condenser pipe (comprising successively air set pipe, 8 ℃ of water condensing tubes, 4 ℃ of water condensing tubes) by the folded band of steam, cooled mushroom essence is mixed the turbid shape liquid that is creamy white with water, enter in the U-shaped pipe of condenser pipe lower end, by U-shaped pipe lower part outlet, can collect and obtain the aqueous natural mushroom essence of milkiness;
Wherein, when mushroom liquor boiling, steam starts, after condensation, to open flow control valve, and the water in water replanishing device is added in mushroom feed liquid; In whole leaching process, adjust flux control valve, controls and to add water speed and distillate to distillate speed consistent.
Adopt each component content in the natural mushroom essence that gas chromatography Detection and Extraction obtain, obtain wherein 1,2,3,5, the yield of 6-five sulphur cycloheptane is 6.9 μ g/g (with mushroom dry weight basis).
The extraction of the natural mushroom essence of embodiment 5
(1) get the cap of dried thin mushroom (kind is the large mushroom of light face), pulverize and sieve, obtain 60 order powder samples, be mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder is placed in 2000ml, add the distilled water of 12 times of weight ratios, mix, obtain mushroom feed liquid.
(3) on there-necked flask, install agitator, synchronous distilling and extracting device (SDE) and water replanishing device;
Wherein, water replanishing device is a leveling bottle, and the water outlet in body side is connected with rubber tube, and rubber tube inserts in there-necked flask after connecting glass tube; Flow control valve is housed on rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 2h, control vapo(u)rizing temperature at 98 ℃, keep the boiling of mushroom feed liquid.In still-process, mushroom essence is entered condenser pipe (comprising successively air set pipe, 8 ℃ of water condensing tubes, 4 ℃ of water condensing tubes) by the folded band of steam, cooled mushroom essence is mixed the turbid shape liquid that is creamy white with water, enter in the U-shaped pipe of condenser pipe lower end, by U-shaped pipe lower part outlet, can collect and obtain the aqueous natural mushroom essence of milkiness.
Wherein, when mushroom liquor boiling, steam starts, after condensation, to open flow control valve, and the water in water replanishing device is added in mushroom feed liquid; In whole leaching process, adjust flux control valve, controls and to add water speed and distillate to distillate speed consistent.
Adopt each component content in the natural mushroom essence that gas chromatography Detection and Extraction obtain, obtain wherein 1,2,3,5, the yield of 6-five sulphur cycloheptane is 11.5 μ g/g (with mushroom dry weight basis).
The impact of embodiment 6-10 solid-liquid ratio on mushroom essence yield
With reference to the method for embodiment 3, in step 2, add the weight ratio of water to be respectively 6,15,20,25 times, in step 4, the heat time is 2h, all the other steps are identical; Measure the yield of 1,2,3,5,6-, five sulphur cycloheptane.Concrete outcome is in Table 3.
The impact of table 3 solid-liquid ratio to 1,2,3,5,6-, five sulphur cycloheptane yield
| Sequence number | Water: the weight ratio of sample | The yield of 1,2,3,5,6-, five sulphur cycloheptane (μ g/g) |
| Embodiment 6 | 6 | 6.7 |
| Embodiment 7 | 10 | 9.6 |
| Embodiment 8 | 15 | 7.0 |
| Embodiment 9 | 20 | 4.5 |
| Embodiment 10 | 25 | 2.1 |
Comprehensive embodiment 6-10 is known, along with the increase of amount of water, has increased the diversity of sample room, and make 1,2,3,5,6-, five sulphur cycloheptane extract content and be significantly increased, at the proportion of water, be that 10 o'clock yield reach maximum 9.6 μ g/g.Afterwards, with the increase of rate of water added, the extraction efficiency of mushroom essence declines, and this may be along with amount of water increases, and the water required heat that seethes with excitement also increases, and causes in same time steam to reduce and make due to its mushroom essence amount of carrying secretly declines.
The impact on mushroom essence yield of embodiment 11-14 extraction time
With reference to the method for embodiment 3, in step 4, the mushroom feed liquid heat time is respectively to 1h, 1.5h, 2h, 3h, all the other steps are identical; Measure the yield of 1,2,3,5,6-, five sulphur cycloheptane.Concrete outcome is in Table 4.
The impact to 1,2,3,5,6-, five sulphur cycloheptane yield of table 4 extraction time
| Sequence number | Time (h) | The yield of 1,2,3,5,6-, five sulphur cycloheptane (μ g/g) |
| Embodiment 11 | 1 | 9.1 |
| Embodiment 12 | 1.5 | 10.7 |
| Embodiment 13 | 2 | 12.6 |
| Embodiment 14 | 3 | 15.0 |
Comprehensive embodiment 3 and embodiment 11-14 are known, and along with the prolongation of extraction time, 1,2,3,5,6-, five sulphur cycloheptane recovery rates are in rising trend.When 2h-2.5h, there is growth trend more stably, during heating 2h 1,2,3,5,6-, five sulphur cycloheptane yield are 12.6 μ g/g, during 2.5h, yield is 13.0 μ g/g, and local flavor is saturated strong, although continue heating, makes 1,2,3,5, the yield of 6-five sulphur cycloheptane further improves, but occurs a small amount of unhappy smell, has destroyed the joyful local flavor of integral body of mushroom essence, and consider energy-conservation needs, will the heat time be controlled at 2-2.5h more satisfactory.
The impact of embodiment 15-19 degree of grinding on mushroom essence yield
With reference to the method for embodiment 3, in step 1, mushroom dry powder degree of grinding is respectively 20 orders, 40 orders, 60 orders, 80 orders, 100 orders, in step 4, to the mushroom feed liquid heat time be 2h, all the other steps are identical; Measure the yield of 1,2,3,5,6-, five sulphur cycloheptane.Concrete outcome is in Table 5.
The impact of table 5 degree of grinding on mushroom essence yield
| Sequence number | Degree of grinding (order) | The yield of 1,2,3,5,6-, five sulphur cycloheptane (μ g/g) |
| Embodiment 15 | 20 | 6.5 |
| Embodiment 16 | 40 | 8.3 |
| Embodiment 17 | 60 | 14.4 |
| Embodiment 18 | 80 | 12.6 |
| Embodiment 19 | 100 | 6.4 |
From embodiment 15-19, sample particle degree is obtained maximum yield when 60 order, and along with order number increases, extraction efficiency is on a declining curve on the contrary afterwards.It is meticulous that the reason that occurs this phenomenon may be that sample is pulverized, affected solvent the flowing of storeroom, and the viscosity suction-operated on volatile ingredient and sample particle surface is strengthened, affect overflowing of volatile ingredient, thereby caused 1,2, the decline of 3,5,6-, five sulphur cycloheptane yield.
Comparative example
With reference to the disclosed method of the people such as Yang Kai, (poplar opens, Sun Peilong, Zheng builds forever etc. a kind of extraction of mushroom essence and constituent analysis, China's flavouring, 2005,6:24-28.) from dried thin mushroom, extract mushroom essence, concrete technology condition is: 50g raw meal is broken to 100 orders, by 1: 15 solid-to-liquid ratio, add in 2L round-bottomed flask, steam distillation is extracted 6h.Distill the 4 ℃ of refrigerations of milky mushroom rectifying lease making that obtain and spend the night, 14000rpm, 15min, 4 ℃ of high speed refrigerated centrifuges are centrifugal, suction pipe carefully sucks supernatant liquor, retain lower floor's milky dirty solution, add again excessive anhydrous sodium sulfate dehydration, 10000rpm, 10min, 4 ℃ after again centrifugal white thick shape mushroom essence crude product, pipette Measurement accuracy volume, V=0.31ml, extracting the thick crude extract volume of gained after the milky mushroom rectifying lease making centrifugal dehydration of gained is 0.31ml, to have comprised 1, 2, 3, 5, 6-five sulphur cycloheptane are at the cumulative volume of the mixture of interior all flavor substances.The average extraction yield that calculates mushroom essence crude product (general volatile flavor substance) is 6.2ml/kg, i.e. 6.2 μ l/g.
Comparative example and comparative example, show to adopt the inventive method can obtain 1,2,3,5 of higher yield, 6-five sulphur cycloheptane, and the flavor substance composition in mushroom essence is abundanter.
Application examples
The mushroom essence product that embodiment 1 is made be take the ratio that weight ratio is 0.2% and is added in the mushroom tartar sauce of making of edodes leftovers, compare with the tartar sauce that does not add mushroom essence, this product fragrance is stronger, and fragrance is lasting, and local flavor is pressed close to natural mushroom boiling local flavor more.
Claims (1)
1. an extracting method for natural mushroom essence, comprising: mushroom (Lentinus edodes Sing.) dry powder is added to the water, and steam distillation is extracted 1-4h, collects distillate, obtains natural mushroom essence;
It is characterized in that, in steam distillation leaching process, in the mixture of mushroom dry powder and water, add water, the described speed of adding water during with steam distillation distillate to distillate speed identical; Described mushroom dry powder obtains by the cap drying of mushroom, after pulverizing; The particle diameter of described mushroom dry powder is 60-100 order; When mushroom dry powder is added to the water, described mushroom dry powder and the weight ratio of water are 1:10-1:12; The vapo(u)rizing temperature of described steam distillation is 95-99 ℃; The time that described steam distillation is extracted is 1.5-2.5h; The condensation of described steam distillation adopts the three step condensation methods that comprise air setting, 8-13 ℃ water condensation, 4-10 ℃ water condensation.
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| CN201210121434.8A CN102657326B (en) | 2012-04-23 | 2012-04-23 | Natural lentmus edodes powder and extracting method and application thereof |
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| RU2514624C1 (en) * | 2013-08-12 | 2014-04-27 | Олег Иванович Квасенков | Method for production of preserves "vegetables and mushrooms salad" |
| CN103750266B (en) * | 2014-02-24 | 2017-01-25 | 云南健牛生物科技有限公司 | Wild mushroom composite seasoning salt and preparation method thereof |
| CN104591968B (en) * | 2015-02-03 | 2016-03-23 | 滕州市悟通香料有限责任公司 | A kind of synthetic method of 1-OCOL |
| CN115399359B (en) * | 2022-10-10 | 2023-04-25 | 丽江三川实业集团有限公司 | Processing device and processing method for ham sausage or sausage containing edible fungi |
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| CN101416721A (en) * | 2008-12-10 | 2009-04-29 | 河南科技学院 | Method for extracting a great variety of biological active ingredients from dry powder of pasania fungus |
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| CN1093881A (en) * | 1993-04-18 | 1994-10-26 | 冯文静 | Herb of Thinleaf GLossogyne products |
| CN101554222A (en) * | 2008-04-10 | 2009-10-14 | 四川省砚山中药饮片有限公司 | Mushroom monosodium glutamate and extraction method thereof |
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