CN113588823A - Method for analyzing flavor contribution of brewing raw materials in Luzhou-flavor liquor - Google Patents
Method for analyzing flavor contribution of brewing raw materials in Luzhou-flavor liquor Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
- C12G3/00—Preparation of other alcoholic beverages
- C12G3/02—Preparation of other alcoholic beverages by fermentation
- C12G3/021—Preparation of other alcoholic beverages by fermentation of botanical family Poaceae, e.g. wheat, millet, sorghum, barley, rye, or corn
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12G—WINE; PREPARATION THEREOF; ALCOHOLIC BEVERAGES; PREPARATION OF ALCOHOLIC BEVERAGES NOT PROVIDED FOR IN SUBCLASSES C12C OR C12H
- C12G3/00—Preparation of other alcoholic beverages
- C12G3/02—Preparation of other alcoholic beverages by fermentation
- C12G3/021—Preparation of other alcoholic beverages by fermentation of botanical family Poaceae, e.g. wheat, millet, sorghum, barley, rye, or corn
- C12G3/022—Preparation of other alcoholic beverages by fermentation of botanical family Poaceae, e.g. wheat, millet, sorghum, barley, rye, or corn of botanical genus Oryza, e.g. rice
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- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12H—PASTEURISATION, STERILISATION, PRESERVATION, PURIFICATION, CLARIFICATION OR AGEING OF ALCOHOLIC BEVERAGES; METHODS FOR ALTERING THE ALCOHOL CONTENT OF FERMENTED SOLUTIONS OR ALCOHOLIC BEVERAGES
- C12H6/00—Methods for increasing the alcohol content of fermented solutions or alcoholic beverages
- C12H6/02—Methods for increasing the alcohol content of fermented solutions or alcoholic beverages by distillation
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- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/62—Detectors specially adapted therefor
- G01N30/72—Mass spectrometers
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- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N30/00—Investigating or analysing materials by separation into components using adsorption, absorption or similar phenomena or using ion-exchange, e.g. chromatography or field flow fractionation
- G01N30/02—Column chromatography
- G01N30/04—Preparation or injection of sample to be analysed
- G01N2030/042—Standards
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Abstract
The invention belongs to the technical field of liquor flavor analysis, and particularly relates to an analysis method for flavor contribution of liquor making raw materials in strong aromatic liquor. The invention aims to solve the technical problem of providing an analysis method for flavor contribution of brewing raw materials in strong aromatic Chinese spirits. The method comprises the following steps: a. collecting distillate or fermentation samples by simulating a collection method or a fermentation method of brewing raw material cooking aroma components in the production process of the strong aromatic Chinese spirits; b. and (c) analyzing the aroma components of the distillate or the fermentation sample collected in the step a. The method is more systematic, closer to the actual production and more suitable for analyzing the flavor of the brewing raw materials of the Luzhou-flavor liquor, provides data support for selection and proportion of the brewing raw materials and provides theoretical basis for improving the quality of the liquor.
Description
Technical Field
The invention belongs to the technical field of liquor flavor analysis, and particularly relates to an analysis method for flavor contribution of liquor making raw materials in strong aromatic liquor.
Background
The white spirit is a traditional Chinese distilled spirit prepared by taking grains as raw materials through the steps of stewing, saccharifying, fermenting, distilling, storing and blending. The grain raw materials for brewing the white spirit are various, wherein sorghum, rice, sticky rice, wheat, corn and highland barley are the most common. The brewing raw material is the first material basis for determining the quality of the white spirit. The liquor world has a statement of 'sorghum produces bouquet, corn produces sweet wine, barley produces brewed wine, glutinous rice produces soft wine, rice produces clean wine, and wheat produces coarse wine'. This fully explains that different raw materials brew white spirit, and the flavor has each characteristic.
The influence of the raw materials on the flavor of the white spirit mainly comes from two aspects: in the production process of the white spirit, the liquor steaming and the grain steaming are always carried out simultaneously, and when grains are steamed and gelatinized, the free aroma substances enter the wine body along with steam, which is the source of 'grain aroma' in the liquor; the grains after being cooked and gelatinized are spread, added with yeast and then fermented in a cellar, wherein macromolecular substances such as starch, protein, fat, tannin and the like generate ethanol and a plurality of flavor substances under the action of microorganisms and enzymes thereof to endow the liquor with special aroma and taste.
There are many reports on the research of the flavor substances of the white spirit at home and abroad, but there is only a report on the research of the influence of the brewing raw materials on the flavor substances of the white spirit. The current research on brewing raw materials mainly focuses on the following 3 aspects: (1) analyzing physical and chemical properties of raw materials; (2) analyzing the cooking aroma components of the grains, such as analyzing the cooking aroma components in 5 brewing raw materials by GC-O-MS (2016) in journal articles of food science; a journal article in food and fermentation industry, wherein the volatile aroma components of cooked sorghum for brewing are analyzed by applying a headspace solid phase microextraction-gas chromatography mass spectrometry technology (2017); the results of these two documents show that: after grains for brewing are cooked, most of aroma components exist in the white spirit, and the composition difference of aroma substances is obvious after different types of brewing raw materials are cooked; (3) analysis of grain fermentation aroma components, for example, in a journal article of food science, namely, analysis of specificity of flavor substances of single-grain white spirit brewed by different brewing raw materials (2019), the result of the article shows that different grains take medium-temperature Daqu as a leavening agent, the type and content of the flavor substances generated by simulated solid state fermentation are greatly different, and the single-grain brewing characteristics are summarized by comprehensive evaluation in three aspects of sensory evaluation, aroma component intensity and aroma substance quantitative analysis, and the conclusion that sorghum is the best brewing raw material is obtained. The research results provide a certain basis for analyzing the flavor substance sources in the white spirit, but the relationship between grains and the flavor of the white spirit cannot be systematically and comprehensively clarified: for example, in the research of grain cooking aroma components, researchers take a small amount (1-5 g) of cooked grains as research objects to explore the aroma components of the cooked grains, but in the actual production, grain cooking and liquor cooking are often performed synchronously in the production process of strong aromatic liquor, grain aroma in the liquor mainly comes from grain cooking aroma components carried out by ethanol in the distillation process, and the research results only carry out qualitative analysis on the cooked grains, namely only explain the problems of grain aroma substances in the liquor, and the content of the flavor substances in the liquor cannot be deeply researched; in the research of grain fermentation aroma components, a method adopted by researchers is a production process of fen-flavor liquor, and qualitative and quantitative results generated by the research can only be used as data support of the fen-flavor liquor.
The research takes single grain as a research object, and the difference of flavor substances generated by steaming and fermenting single grain and multiple grains is not deeply researched. Due to the difference of the raw material proportion and the leavening agent (namely Daqu), the research method and the result have no reference significance to the strong aromatic white spirit, in particular to the multi-grain strong aromatic white spirit. Meanwhile, the research is not combined with the actual production, and the influence of acidity and ethanol content in fermented grains on grain gelatinization effect and steaming aroma in the actual production process of the Luzhou-flavor liquor and the influence of raw material looseness on fermentation effect in the fermentation process are considered.
Disclosure of Invention
In order to solve the defects of the prior art, the invention provides an analysis method for flavor contribution of brewing raw materials in strong aromatic Chinese spirits, which comprises the following steps: a. collecting distillate or fermentation samples by simulating a collection method or a fermentation method of brewing raw material cooking aroma components in the production process of the strong aromatic Chinese spirits; b. and (c) analyzing the aroma components of the distillate or the fermentation sample collected in the step a.
In the step a, the brewing raw materials are single grains or multiple grains.
Further, the single grain is sorghum, rice, glutinous rice, wheat or corn.
Preferably, the single grain is sorghum.
Further, the multi-grain is five grains including sorghum, rice, glutinous rice, wheat and corn.
In the step a, the method for collecting the steam-cooked aroma components of the brewing raw materials comprises the following steps: a pretreatment method and a distillation method of wine brewing raw materials.
Further, in the method for collecting the steam-cooked aroma components of the wine brewing raw material, the pretreatment method of the wine brewing raw material comprises the following steps: a pretreatment method of a steamed wine brewing raw material and a pretreatment method of a wine brewing raw material simulating a production process of strong aromatic Chinese spirits.
Further, the pretreatment method of the steamed wine brewing raw material comprises the following steps: adding water into the crushed wine brewing raw materials to moisten grains and turning and stirring.
Further, the pretreatment method of the brewing raw materials for simulating the production process of the Luzhou-flavor liquor comprises the following steps: adding or not adding 10-20 wt% of cooked bran into the crushed wine brewing raw material, uniformly mixing, adding 60-90 wt% of water equivalent to the dry weight of the raw material, moistening the grains, turning over and stirring, and finally adding lactic acid and ethanol to adjust the acidity and the ethanol content to be similar to those of the wine discharged from the cellar.
Further, in the distillation method, after the pretreated brewing raw material is distilled and condensed, distillate is obtained.
In the step a, the fermentation method for cooking the aroma components of the wine brewing raw material comprises pretreatment and fermentation of the wine brewing raw material.
Further, in the fermentation method for cooking aroma components by using the brewing raw material, the pretreatment of the brewing raw material comprises the following steps: adding or not adding 10-20 wt% of cooked bran into the crushed wine brewing raw material, uniformly mixing, adding water which is 60-90 wt% of the dry weight of the raw material, moistening the grains, turning over and stirring, and cooking the raw material after moistening the grains and cooling to room temperature.
Further, the fermenting comprises simulating a starter fermentation or a starter fermentation for production.
Furthermore, the simulated leavening agent is at least one of a single strain, a compound strain, saccharifying enzyme and yeast.
Further, the fermentation is to add a simulated leavening agent into the brewing raw material which is cooked and aired to room temperature, uniformly stir and put into a fermentation tank with a breather valve, wherein the fermentation temperature range is 28-37 ℃, and the fermentation time is 7-30 days.
Further, the fermentation agent for production is medium-high temperature Daqu used for producing the strong aromatic Chinese spirits.
Further, the fermentation is to add 5-30 wt% of production leaven into the brewing raw material which is cooked and aired to room temperature, to stir uniformly and to put the mixture into a fermentation tank with a breather valve, wherein the fermentation temperature is 28-37 ℃, and the fermentation time is 7-30 days.
In the step b, the aroma analysis method is liquid-liquid extraction, solid-phase extraction or headspace solid-phase microextraction.
Further, the aroma component analysis method uses an isotope internal standard for quantitative analysis.
Has the advantages that:
the invention combines the actual situation in the production, deconstructs the aroma components generated by the brewing raw materials in the strong aromatic Chinese spirits into grain aroma (distillate) and the aroma components generated by fermentation, provides an analysis method for simulating the cooking aroma components of the brewing raw materials in the production process of the strong aromatic Chinese spirits, also provides an analysis method for simulating the grain fermentation aroma components in the production of the strong aromatic Chinese spirits, and provides a systematic research method for systematically researching the contribution of grains to the flavor of the strong aromatic Chinese spirits.
The acidity and ethanol content in fermented grains in the process of steaming strong aromatic Chinese spirits cause different aroma components in strong aromatic Chinese spirits and fen-flavor Chinese spirits due to the pasting effect of grains and the dragging effect of the steaming aroma and the influence of the looseness of raw materials on the fermentation effect in the fermentation process, so that the existing aroma component analysis method of the fen-flavor Chinese spirits is not suitable for aroma component analysis of the strong aromatic Chinese spirits. The single-grain or multi-grain distillate is obtained for analysis by simulating the grain steaming process in the strong aromatic Chinese spirit production process, compared with the qualitative result that the distilled grains can only reflect the free aroma components of the grains, the distillate obtained by distillation can better reflect the quantity ratio relation of the grain aroma substances in the Chinese spirit, and the quantitative result of the method has more significance than the direct analysis of the aroma components of the steamed grains and is more comparable to the grain aroma substances in the Chinese spirit.
Meanwhile, the raw materials selected for producing the strong aromatic Chinese spirits are sorghum and five mixed grains, the difference of microbial systems of the medium-high temperature Daqu used for production and other aromatic Chinese spirits is large, and the flavor substances produced by fermentation are also greatly different, so that the differences of different single-grain and multi-grain flavor substances and fermentation flavor components are transversely compared, a basis is provided for raw material selection of the Chinese spirits, and data support is provided for the proportion of the raw materials in the production of the multi-grain strong aromatic Chinese spirits.
Detailed Description
The acidity and ethanol content in fermented grains in the process of steaming strong aromatic Chinese spirits cause different aroma components in strong aromatic Chinese spirits and fen-flavor Chinese spirits due to the pasting effect of grains and the dragging effect of the steaming aroma and the influence of the looseness of raw materials on the fermentation effect in the fermentation process, so that the existing aroma component analysis method of the fen-flavor Chinese spirits is not suitable for aroma component analysis of the strong aromatic Chinese spirits. In order to overcome the defects of the prior art, the invention provides a method for collecting cooking aroma components of brewing raw materials, a fermentation method and an analysis method of the aroma components, which simulate the production process of strong aromatic Chinese spirits.
The fen-flavor liquor takes sorghum as a raw material, the Luzhou-flavor liquor is divided into a single-grain Luzhou-flavor liquor and a multi-grain Luzhou-flavor liquor, the single-grain Luzhou-flavor liquor is the sorghum, and the multi-grain Luzhou-flavor liquor is mainly five grains including the sorghum, rice, glutinous rice, wheat and corn. Therefore, the brewing raw materials of the invention are single grain or multiple grains. Further, the single grain is sorghum, rice, glutinous rice, wheat or corn. Preferably, the single grain is sorghum. Further, the multi-grain is five grains including sorghum, rice, glutinous rice, wheat and corn.
The method for collecting the steam-cooked aroma components of the brewing raw materials comprises the following steps: a pretreatment method and a distillation method of wine brewing raw materials.
The pretreatment method comprises a pretreatment method of the steamed wine brewing raw material and a pretreatment method of the wine brewing raw material simulating the production process of the Luzhou-flavor liquor. The distillation method comprises a distillation tool and distillation conditions.
The pretreatment method of the steamed wine brewing raw material comprises the following steps: weighing a certain amount of crushed wine brewing raw materials, adding the crushed wine brewing raw materials into a water room temperature condition equivalent to 60-90 wt% of the dry weight of the raw materials, and moistening the grains for 2-24 h, and turning and stirring for 2-3 times.
Furthermore, hot water at 70-80 ℃ is used for reducing the grain moistening time.
The pretreatment method of the brewing raw materials for simulating the production process of the Luzhou-flavor liquor comprises the following steps: weighing a certain amount of crushed wine brewing raw materials, adding 10-20 wt% of cooked bran, uniformly mixing, adding water with the water temperature equivalent to 60-90 wt% of the dry weight of the raw materials, moistening the grains for 2-24 h, turning over and stirring for 2-3 times, and adding a certain amount of lactic acid and ethanol to adjust the acidity and the ethanol content to be similar to those of the wine discharged from the cellar. Particularly, if the interference of the bran shell smell on the grain cooking aroma components is to be eliminated, no bran is added.
The bran hull exists in the fermentation system, and can improve the looseness of fermented grains in the Luzhou-flavor liquor and facilitate the growth of aerobic microorganisms at the early stage of fermentation, so that a certain amount of crushed brewing raw materials are weighed and added with 10-20 wt% of cooked bran.
The fen-flavor liquor is prepared by steaming (namely only steaming grains) raw materials, adding water, cooling, adding yeast, fermenting in a jar (without bran shells in a fermentation system), adding a certain amount of bran, steaming liquor, and discarding lees after the liquor is steamed. The strong aromatic white spirit adopts the processes of mixed steaming, mixed burning and continuous grain fermentation, the mature fermented grains in the previous round of fermentation and the fresh grains in the current round are distilled together, the grains are gelatinized in the distillation process, and meanwhile, the free aroma components in the grains enter the raw spirit under the dragging of ethanol-water vapor, namely the 'grain aroma' substances in the white spirit; the distilled grains have certain free-state and combined-state aroma components, the substances either continue to remain in the fermented grains and enter the wine body along with the next distillation, or are metabolized by microorganisms in the fermentation process of the fermented grains to generate other substances, the distilled grains can only reflect the qualitative result of the free-state aroma components of the grains, and the distillate obtained by distillation can better reflect the quantity ratio relation of the grain aroma components in the white wine. Therefore, the analysis sample of the wine making raw material steam-boiling aroma components is distillate of the pretreated raw material, the distillation device is a small-sized steamer for laboratory (a reduced version of a steamer in a production workshop), and the distillation device consists of a bottom pot, a steamer cover, a gas guide pipe and an ice bucket, and the specific operation steps are as follows: adding sufficient clear water into the bottom pot, introducing condensed water into the ice bucket, uniformly spreading the pretreated raw materials in the steamer, covering the steamer cover, connecting the steamer cover with the ice bucket by using an air duct, placing the electric furnace under the bottom pot, adjusting to proper fire, distilling, and collecting the condensed distillate. The distillate is collected periodically or quantitatively.
The fermentation method of the wine brewing raw material mainly comprises the steps of raw material pretreatment and fermentation conditions, wherein the fermentation conditions comprise simulated starter fermentation and starter fermentation for production.
The raw material pretreatment method comprises the following steps: weighing a certain amount of crushed wine brewing raw materials, adding 10-20 wt% of cooked bran, uniformly mixing, adding water at the temperature of the water, wherein the water is 60-90 wt% of the dry weight of the raw materials, moistening the grains for 2-24 hours, and stirring for 2-3 times during the grain moistening period. Particularly, if the interference of the bran shell smell on the grain cooking aroma components is to be eliminated, no bran is added.
And (3) after the grain moistening is finished, putting the raw materials into the small-sized steamer, steaming for 30-100 min (the steaming time is adjusted according to the amount of the raw materials), and putting the steamed raw materials into a clean tray to cool to room temperature.
The fen-flavor liquor fermentation microorganisms are derived from medium-temperature Daqu, and the Luzhou-flavor liquor fermentation microorganisms are derived from high-temperature Daqu and pit mud, comprise prokaryotic microorganisms and anaerobic microorganisms, and are replaced by composite strains in simulated fermentation. Therefore, the simulated leavening agent is at least one of a single strain, a composite strain, saccharifying enzyme and yeast.
The fermentation conditions were as follows: adding a proper amount of simulated leavening agent (the addition amount is adjusted according to the experimental design) into the raw materials which are aired to the room temperature, uniformly stirring, and then putting into a fermentation tank with a breather valve, wherein the fermentation temperature range is 28-37 ℃, and the fermentation time is 7-30 days.
The starter used for the fen-flavor liquor comprises medium-temperature Daqu, Xiaoqu and bran koji, the strong-flavor liquor mostly uses medium-high temperature Daqu, the difference of microbial systems of the medium-high temperature Daqu used for producing the strong-flavor liquor and other flavor liquor is large, and flavor substances generated by fermentation are also greatly different, so that in order to better simulate the production process of the strong-flavor liquor, the aroma components of the strong-flavor liquor are obtained, the starter used for production is the medium-high temperature Daqu used for producing the strong-flavor liquor, and the fermentation conditions are as follows: adding 5-30 wt% of yeast for production into the raw materials aired to room temperature, uniformly stirring, and then putting into a fermentation tank with a breather valve, wherein the fermentation temperature range is 28-37 ℃, and the fermentation time is 7-30 days.
The analysis samples of the aroma component analysis method are the wine brewing raw material distillate and the solid state fermentation sample.
The aroma component analysis method comprises a liquid-liquid extraction method (LLE), a solid-phase extraction method (SPE) and a headspace solid-phase microextraction method (SPME); the analytical instrument was GC-MS (gas chromatograph-mass spectrometer 7890B-5977B, Agilent, USA).
In particular, the aroma analysis method uses an isotopic internal standard.
The liquid-liquid extraction method (LLE) is mainly used for treating distillate, and the specific method comprises the following steps: weighing a certain amount of distillate into a separating funnel, adding 20-50 mL of extraction liquid, shaking for extraction for 5-10 min, standing for 10-20 min, transferring the extraction liquid into a clean container, repeating the steps for 3 times, combining the extraction liquids, and carrying out nitrogen blowing concentration.
The solid phase extraction method (SPE) adopts a commercial LiChrolut EN solid phase extraction column, the method is used for treating distillate or a solid state fermentation sample, and when the method is used, a sample leaching solution needs to be prepared for the solid state fermentation sample, and the method comprises the following steps: weighing a certain amount of solid state fermentation sample as follows: solution 1: 3-5, adding 3-10% vol ethanol water solution, performing vortex leaching for 5min, and performing high-speed centrifugation to obtain supernatant, namely leaching liquor. The solid phase extraction method comprises the following steps: activating a LiChrollut EN solid-phase extraction column by using dichloromethane, methanol and 3-10% vol ethanol water solution in sequence, then quantitatively adding distillate or leaching liquor into the LiChrollut EN solid-phase extraction column, passing the LiChrollut EN solid-phase extraction column through the column (namely loading), leaching the LiChrollut EN solid-phase extraction column by using 5-10 mL of ultrapure water after loading is finished, and draining at room temperature and adding a certain amount of eluant for elution.
The headspace solid phase microextraction method (SPME) adopts a commercial DVB/CAR/PDMS extraction head, is used for treating distillate or solid fermentation samples, and comprises the following steps: weighing 1-2 g of solid fermentation sample (weighing 1-2 mL of distillate), and directly loading on a headspace bottle for analysis (SPME sample introduction uses a sample pretreatment stage with the parameters of 60 ℃ balance for 15min, 250rpm rotation, 45min extraction and 3min desorption).
The instrumental analysis method is as follows: (different chromatographic columns and instrument parameters are different, and the instrument parameters used in the examples of the application are as follows:
the chromatographic column is a DB-WAXETR chromatographic column;
the carrier gas is He flow rate of 1 mL/min;
the temperature of a sample inlet is 230 ℃;
the temperature raising program of the column box is that the temperature is kept for 5min at 40 ℃ and then is raised to 230 ℃ at 4 ℃/min and kept for 15 min.
In the GC-MS analysis method, EI ionization source electron energy of 70eV, ion source temperature of 230 ℃, quadrupole rod temperature of 150 ℃ and interface temperature of 250 ℃ are adopted for mass spectrum.
Example 1 analysis of steam cooking aroma component in Single-grain and Multi-grain simulation production
Pretreatment of brewing raw materials: weighing 1000g of ground local sorghum, foreign sorghum and five-grain powder respectively, adding 800mL of cold water, moistening the grains for 2h at room temperature, adding 75mL of absolute ethyl alcohol and 100g of lactic acid, and uniformly mixing. After steaming, the raw materials are uniformly spread and sprinkled in the steamer to be steamed for 30min, and condensed distillate (about 500mL) is collected.
Quantitative analysis of aroma substances:
sample treatment: the sample is prepared by using a solid phase extraction method, measuring 50mL of the sample, adding 60 mu L of 50ppm isotope internal standard, swirling for 2-5 min, loading the sample on a Lichroluten small column, eluting with dichloromethane, adding anhydrous sodium sulfate to remove residual moisture, and transferring the liquid into a clean bottle to be subjected to nitrogen blowing. The results of the quantitative analysis of aroma components are shown in table 1 below:
TABLE 1 example 1 quantitative analysis results of aroma components
Example 2 analysis of aroma Components in Single-grain and Multi-grain simulated fermentation
Pretreatment of brewing raw materials: weighing 1000g of the crushed sorghum, rice, sticky rice, wheat, corn and five grains respectively, adding 800mL of hot water, and moistening the grains for 2h at room temperature. After steaming, the raw materials are uniformly spread and sprinkled in the steamer to be steamed for 30 min. Activated dry yeast and 8g of saccharifying enzyme, which are 0.2% of the dry weight of the raw material, are added to the raw material which is cooled to room temperature, and the mixture is stirred uniformly and then put into a fermentation tank with a breather valve, and cultured for 30 days at 30 ℃.
Quantitative analysis of aroma substances:
sample treatment: the test sample treatment uses a solid phase extraction method, 10g of a sample is weighed, 20mL of 3-10% ethanol aqueous solution is added, 500-1000 ppm of mixed isotope internal standard is added, vortex is carried out for 2-5 min, centrifugation is carried out for 10min, the supernatant is put on a Lichroluten small column, dichloromethane is used for elution, anhydrous sodium sulfate is added to remove residual moisture, and liquid is transferred into a clean bottle and is subjected to nitrogen blowing. The results of the quantitative analysis of aroma are shown in Table 2 below:
table 2 example 2 quantitative analysis results of aroma components
Example 3 analysis of aroma Components in Single-grain and Multi-grain Daqu fermentation
Pretreatment of brewing raw materials: weighing 1000g of ground local sorghum, foreign sorghum and five-grain powder respectively, adding 800mL of cold water, adding 100g of bran shells, uniformly mixing, and moistening the grains for 2h at room temperature. After steaming, the raw materials are uniformly spread and sprinkled in the steamer to be steamed for 30 min. Adding middle-high temperature Daqu for production corresponding to 20% of dry weight of the raw materials into the raw materials cooled to room temperature, stirring well, placing into a fermentation tank with a breather valve, and culturing at 30 deg.C for 30 days.
Quantitative analysis of aroma substances:
sample treatment: the sample is prepared by using a headspace solid phase microextraction method, weighing 1g of fermented sample in a headspace bottle, and adding 10 mu L of 100ppm isotope internal standard.
The results of the quantitative analysis of aroma are shown in Table 3 below:
table 3 example 3 quantitative analysis result of aroma component
Claims (10)
1. The method for analyzing the flavor contribution of the brewing raw materials in the Luzhou-flavor liquor is characterized by comprising the following steps of: the method comprises the following steps: a. collecting distillate or fermentation samples by simulating a collection method or a fermentation method of brewing raw material cooking aroma components in the production process of the strong aromatic Chinese spirits; b. and (c) analyzing the aroma components of the distillate or the fermentation sample collected in the step a.
2. The method for analyzing the flavor contribution of the brewing raw material in the Luzhou-flavor liquor, according to claim 1, is characterized in that: in the step a, the method for collecting the steam-cooked aroma components of the brewing raw materials comprises the following steps: a pretreatment method and a distillation method of wine brewing raw materials; the pretreatment method of the brewing raw material comprises the following steps: a pretreatment method of a steamed wine brewing raw material and a pretreatment method of the wine brewing raw material for simulating a production process of the strong aromatic Chinese spirits; in the distillation method, the pretreated brewing raw material is distilled and condensed to obtain distillate.
3. The method for analyzing the flavor contribution of the brewing raw material in the Luzhou-flavor liquor, according to claim 2, is characterized in that: the pretreatment method of the steamed wine brewing raw material comprises the following steps: adding water into the crushed wine brewing raw materials to moisten grains and turning and stirring.
4. The method for analyzing flavor contribution of brewing raw materials in Luzhou-flavor liquor according to claim 2 or 3, wherein the method comprises the following steps: the pretreatment method of the brewing raw materials for simulating the production process of the Luzhou-flavor liquor comprises the following steps: adding or not adding 10-20 wt% of cooked bran into the crushed wine brewing raw material, uniformly mixing, adding 60-90 wt% of water equivalent to the dry weight of the raw material, moistening the grains, turning over and stirring, and finally adding lactic acid and ethanol to adjust the acidity and the ethanol content to be similar to those of the wine discharged from the cellar.
5. The method for analyzing the flavor contribution of the brewing raw material in the Luzhou-flavor liquor, according to claim 1, is characterized in that: in the step a, the fermentation method for cooking the aroma components of the wine brewing raw material comprises pretreatment and fermentation of the wine brewing raw material.
6. The method for analyzing flavor contribution of brewing raw materials in Luzhou-flavor liquor according to claim 5, wherein the method comprises the following steps: the pretreatment of the brewing raw material in the fermentation method for cooking the aroma components of the brewing raw material comprises the following steps: adding or not adding 10-20 wt% of cooked bran into the crushed wine brewing raw material, uniformly mixing, adding water which is 60-90 wt% of the dry weight of the raw material, moistening the grains, turning over and stirring, and cooking the raw material after moistening the grains and cooling to room temperature.
7. The method for analyzing flavor contribution of brewing raw materials in Luzhou-flavor liquor according to claim 5 or 6, wherein the method comprises the following steps: the fermentation comprises simulated fermentation or fermentation of a fermentation agent for production; preferably, the simulated leavening agent is at least one of a single strain, a compound strain, saccharifying enzyme and yeast; the production starter is medium-high temperature Daqu used for producing the strong aromatic Chinese spirits.
8. The method for analyzing the flavor contribution of the brewing raw materials in the Luzhou-flavor liquor according to any one of claims 5 to 7, wherein the method comprises the following steps: and the fermentation is to add a simulated leavening agent or 5-30 wt% of a leavening agent for production into the brewing raw material which is cooked and aired to room temperature, uniformly stir and then put into a fermentation tank with a breather valve, wherein the fermentation temperature range is 28-37 ℃, and the fermentation time is 7-30 days.
9. The method for analyzing the flavor contribution of the brewing raw material in the Luzhou-flavor liquor according to any one of claims 1 to 8, wherein the method comprises the following steps: the brewing raw material is single grain or multiple grains.
10. The method for analyzing the flavor contribution of the brewing raw material in the Luzhou-flavor liquor according to any one of claims 1 to 9, wherein the method comprises the following steps: in the step b, the aroma analysis method is a liquid-liquid extraction method, a solid-phase extraction method or a headspace solid-phase microextraction method; quantitative analysis was performed using isotopic internal standards.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109884213A (en) * | 2019-04-02 | 2019-06-14 | 上海应用技术大学 | A kind of method of quick analysis yellow rice wine key volatile compound |
| CN110358649A (en) * | 2019-08-28 | 2019-10-22 | 北京嘉酿科技有限公司 | A kind of fermentation technique of soft Luzhou-flavor liquo |
| CN110777034A (en) * | 2019-12-09 | 2020-02-11 | 泸州品创科技有限公司 | Strong-flavor highland barley wine and brewing method thereof |
| CN112595786A (en) * | 2020-11-25 | 2021-04-02 | 宜宾五粮液股份有限公司 | Quantitative detection method for volatile flavor substances in fermented grains |
-
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- 2021-07-30 CN CN202110869060.7A patent/CN113588823A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109884213A (en) * | 2019-04-02 | 2019-06-14 | 上海应用技术大学 | A kind of method of quick analysis yellow rice wine key volatile compound |
| CN110358649A (en) * | 2019-08-28 | 2019-10-22 | 北京嘉酿科技有限公司 | A kind of fermentation technique of soft Luzhou-flavor liquo |
| CN110777034A (en) * | 2019-12-09 | 2020-02-11 | 泸州品创科技有限公司 | Strong-flavor highland barley wine and brewing method thereof |
| CN112595786A (en) * | 2020-11-25 | 2021-04-02 | 宜宾五粮液股份有限公司 | Quantitative detection method for volatile flavor substances in fermented grains |
Non-Patent Citations (4)
| Title |
|---|
| ANTONIA TERPOU ET AL: "Entrapped Psychrotolerant Yeast Cells within Pine Sawdust for Low Temperature Wine Making:Impact on Wine Quality", 《MICROORGANISMS》, 20 May 2020 (2020-05-20), pages 1 - 16 * |
| 孙勇民等: "《食品发酵技术》", 中国轻工业出版社, pages: 178 - 181 * |
| 陈果忠 等: "浓香型基础酒和酿造用粮食及大曲的香味成分研究", 《食品工业与科技》 * |
| 陈果忠 等: "浓香型基础酒和酿造用粮食及大曲的香味成分研究", 《食品工业与科技》, 31 December 2018 (2018-12-31), pages 250 - 258 * |
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