CN102657326A - 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 the essence and flavoring agent field, relate in particular to a kind of natural mushroom essence and method for distilling and application.
Background technology
Mushroom (Lentinus edodes Sing.) is a kind of edible mushroom that has long enjoyed a good reputation in China, receives liking of broad masses deeply with the local flavor of its abundant nutrition, uniqueness.Simultaneously, mushroom also is a kind of medicinal fungi, and research in recent years shows that it contains plurality of active ingredients such as lentinan, eritadenine, vitamin and adenosine, has to improve body immunity, antitumor, hypoglycemic, reducing blood lipid and effect such as antiviral.
The peculiar flavour of mushroom is its wide ace-high one big major reason, becomes the focus of Recent study about its check and analysis of volatile ingredient.Research shows, C8 compound is like 1-octene-3-alcohol, 2-octen-1-ol; Sulfur-containing compound comprises 1,2,4-trithio pentamethylene, 1,2,4, and 5-four 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 often being prepared to dried thin mushroom, is eaten, and also drying with it process of the generation of the peculiar flavour of mushroom pleasant is closely related.
Mushroom smart (Lenthionine) is meant 1,2,3,5 on chemical sense, 6-five sulphur cycloheptane, but also can be the general name of volatile flavor substance in the 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 main fragrance component of dried thin mushroom; Its fragrance is strong, and characteristic is strong, is used as main component at present and is widely used in mushroom flavour product and the lenthionine.But current 6-five sulphur cycloheptane are mainly prepared by chemical synthesis process as 1,2,3,5 of product sale, and its fragrance is single, and a perfume (or spice) dashes, but a little less than the body note, whole fragrance is thiner.And tradition is synthetic 1,2,3,5, the method condition of 6-five sulphur cycloheptane harsh (low temperature-78 ℃), and operating process needs through repeatedly extracting, separate, and the reaction time is long, and yield is low.
People such as Yang Kai are raw material with the mushroom; It is smart to adopt steam distillation to extract mushroom; Be specially: confirmed mushroom steam distillation gained general volatile material earlier---the ratio analysis method that mushroom is smart; Confirm that through a plurality of single factor experiments the optimization extraction process condition of the smart steam distillation of mushroom is then: 50g raw material pulverizing to 100 order, add in the 2L round-bottomed flask by 1: 15 solid-to-liquid ratio, steam distillation is extracted 2h.Combine the gas chromatograph-mass spectrometer analysis again, the composition during mushroom rectifying divides under the optimization process conditions is analyzed, (poplar opens to detect 13 kinds of compounds that comprise main taste compound; Sun Peilong, Zheng Jianyong etc. extraction and constituent analysis that a kind of mushroom is smart, Chinese flavouring; 2005,6: 24-28.).This method can be extracted from mushroom and obtain the mushroom essence; But the spectrophotometric detecting method accuracy that it adopted is not high, can not reflect smart each composition of mushroom particularly 1,2 quantitatively; 3; 5, therefore the yield of 6-five sulphur cycloheptane is optimized process conditions according to it and might not be obtained the high product of the smart yield of mushroom; Simultaneously, only detect 13 kinds of compounds in the product that this method makes, composition is less, and it is bigger to extract in the operating process flavor components loss.And document announcement is not seen in the preparation of natural mushroom essence and the quantitative determination of yield thereof at present.
Summary of the invention
The invention provides the smart method for distilling of a kind of natural mushroom, be used for that high yield ground preparation flavor components is many, natural and safe, fragrance mushroom essence true to nature.
The smart method for distilling of a kind of natural mushroom comprises: mushroom (Lentinus edodes Sing.) dry powder is added in the entry, and steam distillation is extracted 1-4h, collects distillate, and it is smart to obtain natural mushroom;
Wherein, in the steam distillation leaching process, in the mixture (being the mushroom feed liquid) of mushroom dry powder and water, add water.
Described mushroom kind is the big mushroom of light face, the little mushroom of light face, Qingyuan 241 or Qingyuan 9015; Be preferably the big mushroom of light face.Different its flavor substances of mushroom kind are little variant, but the general characteristic local flavor is similar, all is with 1,2,3,5, and 6-sulphur cycloheptane is the main contribution composition of the sulfur-containing compound of representative as its characteristic flavor on basis.
Described mushroom dry powder is obtained after drying, pulverizing by mushroom; Preferably, described mushroom dry powder is obtained after drying, pulverizing by the cap of mushroom, and mushroom cap water content is at 8-12%.The flavor substance kind that mushroom cap and bacterium bar are contained, content is difference to some extent all; Sulfur-containing compound and C8 compound that the mushroom local flavor is played main contribution effect etc. mainly concentrates on the cap part; The bacterium bar has then been Duoed some linear paraffins and phenyl ring, heterocyclic compound than cap; This possibly contain more cellulose with the bacterium bar, thereby and suberization takes place causes its flavor components difference relevant.
The particle diameter of described mushroom dry powder is the 60-100 order; Be preferably the 60-80 order; 60 orders more preferably.The purpose of pulverizing is to increase the contact area between feed liquid, and therefore sample is pulverized more carefully well more in theory, and therefore when mushroom dry powder particle diameter was between the 60-100 order, the smart yield of natural mushroom was all higher.It is meticulous that but sample is pulverized, and can influence solvent the flowing of storeroom, and the viscosity suction-operated on volatile ingredient and sample particle surface is strengthened; Influenced overflowing of volatile ingredient; Therefore, when mushroom dry powder particle diameter was 60 orders, the yield of natural mushroom essence was higher.
When adding mushroom dry powder in the entry, the weight ratio of described mushroom dry powder and water is 1: 10-1: 12; Be preferably 1: 10.Increase the water yield, the required heat of water boiling also increases during heating, thereby causes the steam of evaporation in the identical time to reduce, and is also reduced by the smart total amount of its mushroom of carrying secretly.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 low excessively, is unfavorable for that water is carried volatile materials secretly to steam; And vapo(u)rizing temperature is too high, and hydrolysis, oxidation, esterification or thermal decomposition can take place the part volatile materials, even decomposes the material that the little molecule meeting cross reaction generation that obtains influences local flavor.Mushroom dry powder is with after water mixes, and boiling point descends, and is lower than the boiling point (100 ℃) of pure water, adopts 95-99 ℃ vapo(u)rizing temperature, can make the mushroom feed liquid keep boiling, can reduce the loss of volatile materials again, the while energy efficient.
The extraction time of described steam distillation is preferably 1.5-2.5h; 2-2.5h more preferably.In the certain limit, prolong extraction time and help steaming of volatile flavor substance; But overlong time is unfavorable for the needs of energy savings, and along with the prolongation of heat time heating time, can generate some and destroy the natural flavour mountaineous new component of mushrooms, and the overall quality of product is exerted an influence.
The three step condensation methods that comprise air setting, 8-13 ℃ water condensation, 4-10 ℃ water condensation are adopted in the condensation of described steam distillation.Three step condensation methods carry out condensation with the mode that temperature reduces step by step to distillate, can cool off the flavor substance that evaporates more quickly, reduce their volatilization loss, and make the flavor substance that obtains more complete, press close to the local flavor of natural mushroom.
The device of described steam distillation can adopt synchronous distilling and extracting device (SDE), and distilling and extracting device good reproducibility, recovery rate height can be realized three step condensations to distillate synchronously, are particularly suitable for the extraction of volatile materials.Smart in order to obtain directly available natural mushroom, do not use the organic matter extraction part in the synchronous distilling and extracting device, and only use its steam distillation part.
When steam distillation was extracted, moisture steamed gradually, is collected with condensation with mushroom is single-minded, causes the water in the mushroom feed liquid to reduce gradually, influenced the smart extraction efficiency of mushroom; In the mushroom feed liquid, add water in time, continuously, sufficient moisture can be provided, thereby keep the smart extraction efficiency of mushroom in higher level.
Preferably, the described speed of adding water during with steam distillation the speed that distillates of distillate identical, can make the mushroom feed liquid keep suitable solid-liquid ratio so always, guarantee fully steaming of volatile flavor substance.
Preferably, adopt the water replanishing device be connected with the steam distillation device to add water for the mushroom feed liquid, the speed of adding water is controlled through being arranged between steam distillation device and the water replanishing device flow control valve on the tube connector, and precise control is easy to operate.
Smart in order to obtain the higher natural mushroom of concentration, can carry out centrifugal treating to the distillate that collection obtains, get precipitum after finishing dealing with, it is smart to obtain described natural mushroom.Adopt centrifugal treating, can farthest reduce the volatilization of flavor components.
The smart method for distilling of above-mentioned natural mushroom can carry out at mushroom comprehensive processing and utilization pretreatment stage; As when extracting functional components lentinan in the mushroom, eritadenine, mushroom peptide etc.; All can carry out water heating lixiviate of the present invention to the mushroom sample early stage handles; In this processing procedure, collect the mushroom flavor components because of heated volatile, it is smart to obtain natural mushroom, can improve the added value and the comprehensive utilization ratio of mushroom greatly.
It is smart to the invention provides a kind of natural mushroom that adopts the said extracted method to obtain.This natural mushroom essence is the turbid shape liquid of milky, does not contain any organic solvent, is aliment security level.Evidence is the natural mushroom essence that raw material makes with the dried thin mushroom cap, wherein contains more than 30 kind of flavor substance, comprises more than ten kind of sulfur-containing compound (relative amount reaches about 23%), and fragrance is abundant, and is with rich flavor, near dried thin mushroom fragrance.
The present invention also provides the application of above-mentioned natural mushroom essence in preparation mushroom flavour product.This natural mushroom essence is a water extract, does not contain organic solvent, and security is good, can directly or process to add in product or the food behind the condiment to be used for blending, is particularly useful for making homely delicate flavour condiment, mushroom sauce, or the blending of canned mushroom, instant food.
The present invention is raw material with the dried thin mushroom, adopts steam distillation and moisturizing operation to match, and through suitable technological process and technological parameter, extracts and has obtained natural mushroom essence.
Adopt the inventive method, have following beneficial effect:
(1) it is synthetic 1,2,3,5 to compare the traditional chemical method, 6-five sulphur cycloheptane, characteristics such as it is simple that the inventive method has technology, and the reaction time is short, and energy consumption is low, and cost is low.
(2) adopt the inventive method, the smart extraction efficiency of natural mushroom is high, and particularly 1; 2,3,5; 6-five sulphur cycloheptane; Its yield can reach 13.5 μ g/g (with the mushroom dry weight basis), is the at present known smart quantification of unique mushroom that appears in the newspapers 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; Be water extract, do not contain organic solvent, be aliment security level, can directly or process to add to behind the condiment and be used for blending in the product, 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; Promptly carry out flooding of the present invention in earlier stage in functional components such as extracting lentinan, eritadenine, champignon polypeptide; But the mushroom flavor components of synchronous collection volatilization has improved the added value and the comprehensive utilization ratio of mushroom greatly.
Description of drawings
Fig. 1 is that raw material extracts the volatile ingredient TIC that the mushroom essence obtain obtains through the GC-MS check and analysis for the embodiment of the invention 1 with the dried thin mushroom cap.
Fig. 2 is that raw material extracts the volatile ingredient TIC that the mushroom essence obtain obtains through the GC-MS check and analysis for the embodiment of the invention 2 with dried thin mushroom bacterium bar.
The specific embodiment
The smart extraction of embodiment 1 natural mushroom
(1) get the cap of dried thin mushroom (kind is the big mushroom of light face), crushing screening obtains 60 order powder samples, is mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder places 2000ml, add the distilled water of 10 times of weight ratios, mixing obtains the 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, is connected with rubber tube at the delivery port place of body side, and rubber tube inserts in the there-necked flask after connecting glass tube; Flow control valve is housed on the rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 2h, the control vapo(u)rizing temperature keeps the boiling of mushroom feed liquid at 99 ℃.In still-process; The mushroom essence is got into condenser pipe (comprising air set pipe, 8 ℃ of water condensing tubes, 4 ℃ of water condensing tubes successively) by the folded band of steam; The smart turbid shape liquid that is creamy white that mixes with water of cooled mushroom; Get in the U type pipe of condenser pipe lower end, can collect through U type pipe lower part outlet and obtain the aqueous natural mushroom essence of milkiness.
Wherein,, after steam begins condensation, open flow control valve, the water in the water replanishing device is added in the mushroom feed liquid when the boiling of mushroom liquid; In the whole leaching process, regulate flow control valve, control adds water speed and distillate, and to distillate speed consistent.
With the dipropyl disulfide is internal standard compound, sets up the gas-chromatography detection method of the smart content of mushroom, and 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 the mushroom dry weight basis).
Adopt the analysis of GC-MS method to extract in the natural mushroom essence that obtains to become to be grouped into, draw: volatile ingredient identifies 36 kinds altogether, and 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 (is raw material with the dried thin mushroom cap)
The smart extraction of embodiment 2 natural mushrooms
(1) get the bacterium bar of dried thin mushroom (kind is the big mushroom of light face), crushing screening obtains 60 order powder samples, is mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder places 2000ml, add the distilled water of 10 times of weight ratios, mixing obtains the 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, is connected with rubber tube at the delivery port place of body side, and rubber tube inserts in the there-necked flask after connecting glass tube; Flow control valve is housed on the rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 2h, the control vapo(u)rizing temperature keeps the boiling of mushroom feed liquid at 99 ℃.In still-process; The mushroom essence is got into condenser pipe (comprising air set pipe, 8 ℃ of water condensing tubes, 4 ℃ of water condensing tubes successively) by the folded band of steam; The smart turbid shape liquid that is creamy white that mixes with water of cooled mushroom; Get in the U type pipe of condenser pipe lower end, can collect through U type pipe lower part outlet and obtain the aqueous natural mushroom essence of milkiness.
Wherein,, after steam begins condensation, open flow control valve, the water in the water replanishing device is added in the mushroom feed liquid when the boiling of mushroom liquid; In the whole leaching process, regulate flow control valve, control adds water speed and distillate, and to distillate speed consistent.
Adopt the analysis of GC-MS method to extract in the natural mushroom essence that obtains to become to be grouped into; Draw: volatile ingredient identifies 63 kinds altogether, and wherein sulfur-containing compound has 11 kinds, though relative amount 3.381% visible on the 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 contribution composition of dried thin mushroom flavour, and all kinds volatile ingredient is more in the mushroom bacterium bar, comprises some linear paraffins and phenyl ring, heterocyclic compound; This possibly contain more cellulose with the bacterium bar, and maybe 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 that choosing the mushroom cap has more advantage as extracting the smart raw material of mushroom.Mushroom bacterium bar volatile ingredient TIC is seen Fig. 2.
Composition in the natural mushroom essence of table 2 (is raw material with dried thin mushroom bacterium bar)
The smart extraction of embodiment 3 natural mushrooms
(1) get the cap of dried thin mushroom (kind for Qingyuan 241), crushing screening obtains 80 order powder samples, is mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder places 2000ml, add the distilled water of 10 times of weight ratios, mixing obtains the 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, is connected with rubber tube at the delivery port place of body side, and rubber tube inserts in the there-necked flask after connecting glass tube; Flow control valve is housed on the rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 2.5h, the control vapo(u)rizing temperature keeps the boiling of mushroom feed liquid at 97 ℃.In still-process; The mushroom essence is got into condenser pipe (comprising air set pipe, 10 ℃ of water condensing tubes, 6 ℃ of water condensing tubes successively) by the folded band of steam; The smart turbid shape liquid that is creamy white that mixes with water of cooled mushroom; Get in the U type pipe of condenser pipe lower end, can collect through U type pipe lower part outlet and obtain the aqueous natural mushroom essence of milkiness.
Wherein,, after steam begins condensation, open flow control valve, the water in the water replanishing device is added in the mushroom feed liquid when the boiling of mushroom liquid; In the whole leaching process, regulate flow control valve, control adds water speed and distillate, and to distillate speed consistent.
Adopt each component content in the natural mushroom essence that the 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 the mushroom dry weight basis).
The smart extraction of embodiment 4 natural mushrooms
(1) get the cap of dried thin mushroom (kind is the little mushroom of light face), crushing screening obtains 100 order powder samples, is mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder places 2000ml, add the distilled water of 12 times of weight ratios, mixing obtains the 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, is connected with rubber tube at the delivery port place of body side, and rubber tube inserts in the there-necked flask after connecting glass tube; Flow control valve is housed on the rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 1.5h, the control vapo(u)rizing temperature keeps the boiling of mushroom feed liquid at 99 ℃.In still-process; The mushroom essence is got into condenser pipe (comprising air set pipe, 8 ℃ of water condensing tubes, 4 ℃ of water condensing tubes successively) by the folded band of steam; The smart turbid shape liquid that is creamy white that mixes with water of cooled mushroom; Get in the U type pipe of condenser pipe lower end, can collect through U type pipe lower part outlet and obtain the aqueous natural mushroom essence of milkiness;
Wherein,, after steam begins condensation, open flow control valve, the water in the water replanishing device is added in the mushroom feed liquid when the boiling of mushroom liquid; In the whole leaching process, regulate flow control valve, control adds water speed and distillate, and to distillate speed consistent.
Adopt each component content in the natural mushroom essence that the 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 the mushroom dry weight basis).
The smart extraction of embodiment 5 natural mushrooms
(1) get the cap of dried thin mushroom (kind is the big mushroom of light face), crushing screening obtains 60 order powder samples, is mushroom dry powder.
(2) get the there-necked flask that 30g (dry weight) mushroom dry powder places 2000ml, add the distilled water of 12 times of weight ratios, mixing obtains the 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, is connected with rubber tube at the delivery port place of body side, and rubber tube inserts in the there-necked flask after connecting glass tube; Flow control valve is housed on the rubber tube; The distilled water of certain volume is housed in leveling bottle.
(4) to there-necked flask heating 2h, the control vapo(u)rizing temperature keeps the boiling of mushroom feed liquid at 98 ℃.In still-process; The mushroom essence is got into condenser pipe (comprising air set pipe, 8 ℃ of water condensing tubes, 4 ℃ of water condensing tubes successively) by the folded band of steam; The smart turbid shape liquid that is creamy white that mixes with water of cooled mushroom; Get in the U type pipe of condenser pipe lower end, can collect through U type pipe lower part outlet and obtain the aqueous natural mushroom essence of milkiness.
Wherein,, after steam begins condensation, open flow control valve, the water in the water replanishing device is added in the mushroom feed liquid when the boiling of mushroom liquid; In the whole leaching process, regulate flow control valve, control adds water speed and distillate, and to distillate speed consistent.
Adopt each component content in the natural mushroom essence that the 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 the mushroom dry weight basis).
Embodiment 6-10 solid-liquid ratio is to the influence of the smart yield of mushroom
With reference to the method for embodiment 3, in the step 2, the weight ratio that adds entry is respectively 6,15,20,25 times, and in the step 4, be 2h heat time heating time, and all the other steps are identical; Measure 1,2,3,5, the yield of 6-five sulphur cycloheptane.Concrete outcome is seen table 3.
Table 3 solid-liquid ratio is to 1,2,3,5, the influence of 6-five sulphur cycloheptane yield
Sequence number | Water: the weight ratio of sample | 1,2,3,5, the yield of 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 can know, along with the increase of amount of water, has increased the diversity of sample room, makes 1,2,3,5, and 6-five sulphur cycloheptane extract content has obvious increase, is that 10 o'clock yield reach maximum 9.6 μ g/g at the proportion of water.Afterwards, with the increase of rate of water added, the extraction efficiency decline of mushroom essence, this possibly be along with amount of water increases, the required heat of water boiling also increases, due to causing the interior steam minimizing of identical time and its mushroom of carrying secretly essence is measured descending.
Embodiment 11-14 extraction time is to the influence of the smart yield of mushroom
With reference to the method for embodiment 3, in the step 4, the mushroom feed liquid is respectively 1h heat time heating time, 1.5h, 2h, 3h, all the other steps are identical; Measure 1,2,3,5, the yield of 6-five sulphur cycloheptane.Concrete outcome is seen table 4.
Table 4 extraction time is to 1,2,3,5, the influence of 6-five sulphur cycloheptane yield
Sequence number | Time (h) | 1,2,3,5, the yield of 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 |
Comprehensively embodiment 3 and embodiment 11-14 can know, along with the prolongation of extraction time, and 1,2,3,5,6-five sulphur cycloheptane recovery rates are in rising trend.Growth trend more stably appears when 2h-2.5h, when heating 2h 1,2,3,5; 6-five sulphur cycloheptane yield are 12.6 μ g/g, and yield is 13.0 μ g/g during 2.5h, and local flavor is saturated strong, make 1 though continue heating; 2,3,5, the yield of 6-five sulphur cycloheptane further improves; But a small amount of unhappy smell occurs, destroyed the smart whole joyful local flavor of mushroom, and considered energy-conservation needs, it is more satisfactory to be controlled at 2-2.5h heat time heating time.
Embodiment 15-19 degree of grinding is to the influence of the smart yield of mushroom
With reference to the method for embodiment 3, in the step 1, mushroom dry powder degree of grinding is respectively 20 orders, 40 orders, 60 orders, 80 orders, 100 orders, in the step 4, to mushroom feed liquid heat time heating time be 2h, all the other steps are identical; Measure 1,2,3,5, the yield of 6-five sulphur cycloheptane.Concrete outcome is seen table 5.
Table 5 degree of grinding is to the influence of the smart yield of mushroom
Sequence number | Degree of grinding (order) | 1,2,3,5, the yield of 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 |
Can be known that by embodiment 15-19 the sample particle degree is obtained maximum yield when 60 orders, along with the order number increases, extraction efficiency is on a declining curve on the contrary afterwards.It is meticulous that the reason that this phenomenon occurs possibly be that sample is pulverized, influenced solvent the flowing of storeroom, and the viscosity suction-operated on volatile ingredient and sample particle surface is strengthened; Influence overflowing of volatile ingredient, thereby caused 1,2; 3,5, the decline of 6-five sulphur cycloheptane yield.
Comparative Examples
With reference to people's disclosed methods such as Yang Kai (poplar opens, Sun Peilong, Zheng Jianyong etc. extraction and constituent analysis that a kind of mushroom is smart; China's flavouring; 2005,6:24-28.) from dried thin mushroom, extract the mushroom essence, concrete process conditions are: 50g raw material pulverizing to 100 order; Add in the 2L round-bottomed flask by 1: 15 solid-to-liquid ratio, 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; The careful suction of suction pipe removed supernatant liquor, keeps the muddy liquid of lower floor's milky, adds excessive anhydrous sodium sulfate dehydration again, 10000rpm; 10min, 4 ℃ after centrifugal once more the smart bullion of white thick shape mushroom, the accurate measurement volumes of pipette, V=0.31ml; Extracting promptly that the thick crude extract volume of gained is 0.31ml after the milky mushroom rectifying lease making centrifugal dehydration of gained, is to have comprised 1,2; 3,5,6-five sulphur cycloheptane are at the cumulative volume of the mixture of all interior flavor substances.The average extraction yield that calculates the smart bullion of mushroom (general volatile flavor substance) is 6.2ml/kg, i.e. 6.2 μ l/g.
Comparative example and Comparative Examples show and adopt the inventive method can obtain 1,2,3,5 of higher yield, 6-five sulphur cycloheptane, and the flavor substance composition in the mushroom essence is abundanter.
Application examples
The smart product of the mushroom that embodiment 1 is made is that 0.2% ratio is added in the mushroom tartar sauce with the mushroom leftover bits and pieces with weight ratio; The tartar sauce smart with not adding mushroom compared; This product fragrance is stronger, and fragrance is lasting, and local flavor is pressed close to natural mushroom boiling local flavor more.
Claims (10)
1. method for distilling that natural mushroom is smart, comprising: mushroom (Lentinus edodes Sing.) dry powder is added in the entry, and steam distillation is extracted 1-4 h, collects distillate, and it is smart to obtain natural mushroom;
It is characterized in that, in the steam distillation leaching process, in the mixture of mushroom dry powder and water, add water.
2. method for distilling according to claim 1 is characterized in that: described mushroom dry powder is obtained after drying, pulverizing by the cap of mushroom.
3. method for distilling according to claim 1 is characterized in that: the particle diameter of described mushroom dry powder is the 60-100 order.
4. method for distilling according to claim 1 is characterized in that: when adding mushroom dry powder in the entry, the weight ratio of described mushroom dry powder and water is 1: 10-1: 12.
5. method for distilling according to claim 1 is characterized in that: the vapo(u)rizing temperature of described steam distillation is 95-99 ℃.
6. method for distilling according to claim 1 is characterized in that: the time that described steam distillation is extracted is 1.5-2.5h.
7. method for distilling according to claim 1 is characterized in that: the three step condensation methods that comprise air setting, 8-13 ℃ water condensation, 4-10 ℃ water condensation are adopted in the condensation of described steam distillation.
8. method for distilling according to claim 1 is characterized in that: the described speed of adding water during with steam distillation the speed that distillates of distillate identical.
9. the natural mushroom that obtains of employing such as the arbitrary described method for distilling of claim 1-8 is smart.
10. the application of natural mushroom essence as claimed in claim 9 in preparation mushroom flavour product.
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RU2514624C1 (en) * | 2013-08-12 | 2014-04-27 | Олег Иванович Квасенков | Method for production of preserves "vegetables and mushrooms salad" |
CN103750266A (en) * | 2014-02-24 | 2014-04-30 | 云南健牛生物科技有限公司 | Wild mushroom composite seasoning salt and preparation method thereof |
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CN115399359A (en) * | 2022-10-10 | 2022-11-29 | 丽江三川实业集团有限公司 | Processing device and processing method for ham sausages or sausages containing edible fungi |
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Cited By (5)
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RU2514624C1 (en) * | 2013-08-12 | 2014-04-27 | Олег Иванович Квасенков | Method for production of preserves "vegetables and mushrooms salad" |
CN103750266A (en) * | 2014-02-24 | 2014-04-30 | 云南健牛生物科技有限公司 | Wild mushroom composite seasoning salt and preparation method thereof |
CN104591968A (en) * | 2015-02-03 | 2015-05-06 | 滕州市悟通香料有限责任公司 | Synthesis method of 1-octylene-3-alcohol |
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 |
CN115399359A (en) * | 2022-10-10 | 2022-11-29 | 丽江三川实业集团有限公司 | Processing device and processing method for ham sausages or sausages containing edible fungi |
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