CN112175779A - White spirit based on ultrasonic wave and ultraviolet light synergistic ripening acceleration and ripening acceleration method and metabolic flux analysis method thereof - Google Patents
White spirit based on ultrasonic wave and ultraviolet light synergistic ripening acceleration and ripening acceleration method and metabolic flux analysis method thereof Download PDFInfo
- Publication number
- CN112175779A CN112175779A CN202011017253.1A CN202011017253A CN112175779A CN 112175779 A CN112175779 A CN 112175779A CN 202011017253 A CN202011017253 A CN 202011017253A CN 112175779 A CN112175779 A CN 112175779A
- Authority
- CN
- China
- Prior art keywords
- white spirit
- ultraviolet light
- ripening
- ultrasonic wave
- mobile phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
- C12H1/12—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
- C12H1/16—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation
- C12H1/165—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation by irradiation
-
- C—CHEMISTRY; METALLURGY
- 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
- C12H1/00—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages
- C12H1/12—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation
- C12H1/16—Pasteurisation, sterilisation, preservation, purification, clarification, or ageing of alcoholic beverages without precipitation by physical means, e.g. irradiation
-
- 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
-
- 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
- G01N30/04—Preparation or injection of sample to be analysed
- G01N30/06—Preparation
-
- 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
- G01N30/26—Conditioning of the fluid carrier; Flow patterns
- G01N30/28—Control of physical parameters of the fluid carrier
- G01N30/34—Control of physical parameters of the fluid carrier of fluid composition, e.g. gradient
-
- 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
- G01N30/86—Signal analysis
- G01N30/8675—Evaluation, i.e. decoding of the signal into analytical information
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/50—Improvements relating to the production of bulk chemicals
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
Landscapes
- Health & Medical Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Physics & Mathematics (AREA)
- Organic Chemistry (AREA)
- Toxicology (AREA)
- Food Science & Technology (AREA)
- Bioinformatics & Cheminformatics (AREA)
- General Engineering & Computer Science (AREA)
- Genetics & Genomics (AREA)
- Wood Science & Technology (AREA)
- Zoology (AREA)
- Library & Information Science (AREA)
- Other Investigation Or Analysis Of Materials By Electrical Means (AREA)
Abstract
The invention relates to a white spirit based on ultrasonic wave and ultraviolet light ripening acceleration and a ripening acceleration method and a metabolic flux analysis method thereof, wherein the ripening acceleration method comprises the steps of simultaneously carrying out ultraviolet light and ultrasonic wave treatment on new wine under the following conditions to obtain the white spirit subjected to ripening acceleration; the wavelength of the ultraviolet light is 350-385nm, and the power is 180-220W; the frequency of the ultrasonic wave is 20-30kHz, and the power is 100-450W. The metabolic flux analysis method comprises the steps of 1, filtering white spirit by using an organic phase microporous filter membrane, performing data acquisition by adopting ultra-high performance phase combination chromatography-quadrupole time-of-flight mass spectrometry to obtain an original data file, and 2, extracting the original data file and generating a peak table; and 3, normalizing and scaling the retention time of the metabolites in the peak table, the accurate mass of the ion peak, the fragment ion peak intensity and the fragment isotope peak intensity, and then deriving the normalized and scaled fragments and carrying out visualization operation.
Description
Technical Field
The invention relates to the technical field of metabolic flux analysis, in particular to white spirit based on ultrasonic wave and ultraviolet light synergistic ripening acceleration, a ripening acceleration method and a metabolic flux analysis method thereof.
Background
Newly produced white spirit is spicy, violent in brewing and inconsistent in taste, after being aged for a period of time, the mixed taste of the pathogenic factors can be slowly weakened, and the taste of the white spirit is mellow and soft. The most common mode is natural aging, but the traditional aging mode is too much to meet the huge market demand with the continuous expansion of the white spirit market because the natural aging needs a lot of time, the storage needs corresponding capital equipment investment, and the wine consumption loss is added.
Based on the reasons, some artificial ripening accelerating methods appear in recent years, so that the ripening time is shortened, the market supply is met, and the economic benefit of enterprises is increased. However, many complex physicochemical changes occur in the aging process of white spirit, the types of molecules participating in the reaction reach thousands, and the chemical reaction processes and the required reaction energy are different. Therefore, any single aging accelerating technology cannot realize the complete aging of the white spirit, so the combined aging accelerating technology is an effective method for realizing the complete aging of the white spirit.
Ultrasonic wave and ultraviolet irradiation technologies have attracted attention as a distilled liquor ripening means, and whether the ultrasonic wave and the ultraviolet irradiation technologies have a synergistic ripening acceleration effect on white spirit or not has no related report at present. Meanwhile, after ripening treatment, related chemical component analysis and substance change in a white spirit system need to be monitored, so that white spirit with stable quality is produced, metabolic flux analysis is used as a comprehensive and effective method for analyzing the substance change in the sample system, and a non-targeting method is generally adopted as a research starting point to carry out unbiased detection on all components. Then, a corresponding non-targeted analysis model is constructed by a multivariate dimension-reduction statistical method, characteristic compounds with group difference are screened out and characterized, and the method can be effectively used for identifying the variety quality, the production area traceability, the biological activity, the food quality safety, the nutrition control and the like of samples, so that the method is suitable for analyzing related chemical components and monitoring the substance change in a liquor system after ripening treatment, and at present, no related report of metabolic flux analysis after ultrasonic wave and ultraviolet light irradiation of the liquor exists.
Disclosure of Invention
Based on the defects of the prior art, the invention provides white spirit based on ultrasonic wave and ultraviolet light ripening acceleration, a ripening acceleration method and a metabolic flux analysis method thereof, wherein the metabolic flux analysis method is combined with ultra-high performance phase-combination chromatography-quadrupole time-of-flight mass spectrometry (UPC)2QTOF/MS) technology, which not only analyzes the material change in the white spirit system after ripening under the synergistic effect of ultraviolet light and under different ultrasonic conditions and by the ultrasonic wave and ultraviolet light cooperating technology, but also explores the mechanism of accelerating the white spirit ripening by the ultrasonic wave and ultraviolet light cooperating technology, and finally can produce white spirit with stable quality in a shorter time.
The invention is realized by the following technical scheme:
a method for accelerating the ripening of white spirit based on ultrasonic wave and ultraviolet light comprises the following steps of simultaneously carrying out ultraviolet light and ultrasonic wave treatment on new white spirit under the following conditions to obtain the white spirit after the ripening treatment;
the wavelength of the ultraviolet light is 350-385nm, and the power is 180-220W; the frequency of the ultrasonic wave is 20-30kHz, and the power is 100-450W.
Preferably, the new wine is subjected to both ultraviolet light and ultrasonic treatment at 25-35 deg.C.
Preferably, the new wine is treated by ultraviolet light and ultrasonic wave for 15-30 min.
Preferably, the fresh wine is stored in the dark at room temperature for at least 15 days after being subjected to the ultraviolet light and ultrasonic wave treatment under the conditions.
White spirit obtained by the method for ripening white spirit based on ultrasonic wave and ultraviolet light.
A method for analyzing metabolic flux of white spirit based on ultrasonic wave and ultraviolet light synergistic ripening comprises the following steps:
step 1, filtering white spirit by using an organic phase microporous filter membrane, and performing data acquisition by adopting ultra-high performance combined chromatography-quadrupole time-of-flight mass spectrometry to obtain an original data file, wherein the conditions of chromatography and mass spectrometry are as follows;
the chromatographic column is Waters Acquity UPC2CSH Fluoro-phenyl with column temperature of 34-36 deg.C, sample plate temperature of 3-5 deg.C, and supercritical CO as mobile phase A2The mobile phase B is a mixed solution of methanol and acetonitrile, the volume ratio of the methanol to the acetonitrile is 1:1, the back pressure is 12.00-14.00MPa, and the flow rate is 0.4-0.6 mL/min;
the ion source is an electrospray ion source, the capillary voltage is 3.0-5.0kV, the taper hole voltage is 35-40V, the ion source compensation voltage is 80-85V, and the ion source temperature is 110-130 ℃; the temperature of the atomizing gas is 450-500 ℃, the airflow speed of the atomizing gas is 750-800L/h, and the airflow speed of the taper hole is 45-50L/h;
and 3, normalizing and scaling the retention time of the metabolites in the peak table, the accurate mass of the ion peak, the fragment ion peak intensity and the fragment isotope peak intensity, and then exporting to obtain a csv file, and performing visual operation on the csv file to finish the analysis of the metabolic flux of the white spirit based on ultrasonic wave and ultraviolet light synergistic ripening.
Further, in step 1, mobile phase a and mobile phase B are performed by gradient elution: the volume proportion of the mobile phase B is linearly increased from 2 percent to 4 percent within 0-1 min; the volume proportion of the mobile phase B is kept to be 4 percent within 1-6 min; the volume proportion of the mobile phase B is linearly increased to 10 percent from 4 percent within 6 to 6.5 min; the volume proportion of the mobile phase B is kept to be 10 percent within 6.5-14.5 min; the volume proportion of the mobile phase B is linearly reduced from 10 percent to 2 percent within 14.5-15 min.
Further, in the step 1, the scanning mode of the mass spectrum is ESI positive ions/ESI negative ions, and the scanning mode is Full Scan/MSE，MS1And MS2The scanning range is m/z is 100-.
Further, step 2 is to perform noise filtering, smooth integration, background drift, peak extraction and peak alignment on the raw data file, then identify the compound and align it with ddMS2All compounds of the data were subjected to a similarity search, generating a peak table.
Compared with the prior art, the invention has the following advantages:
the invention relates to a method for accelerating the ripening of white spirit based on ultrasonic wave and ultraviolet light, which adopts a combined aging accelerating technology of ultrasonic wave with certain wavelength and power and ultraviolet light irradiation with certain frequency and power, can effectively overcome the phenomenon of the reversion of the white spirit, organic molecular groups in new white spirit absorb ultraviolet energy, so that molecular potential energy is increased, high-energy bond positions among molecules are broken and recombined, and the rate of oxidation, esterification and condensation self-polymerization chemical reactions among the molecules is increased, thereby greatly accelerating the chemical change process of the white spirit. The ultrasonic treatment can enhance the molecular activation of various substances, improve the effective collision rate among molecules, further accelerate the esterification, condensation and oxidation reduction reaction, and is favorable for forming the fragrance of the brewed alcohol ester of the white spirit. Meanwhile, the ultrasonic wave can increase the affinity among polar molecules such as water, alcohol, aldehyde, acid, ester and the like, enhance the association degree of ethanol and water molecules, form large and firm polar molecule association groups, reduce the stimulation of the polar molecule association groups on taste organs and ensure that the wine body gradually becomes soft from burst hot. In addition, the molecular kinetic energy can be increased by ultrasonic, when the ultraviolet frequency is consistent with the stretching vibration frequency which can characterize the characteristic group frequency in the groups (C-H, O-H, C-O, C ═ O) of the functional groups of main components of the wine, such as aldehyde, alcohol, acid, ester and the like, resonance absorption can be generated, the characterized energy can excite organic molecules, so that the organic molecules can generate strong vibration and rotation, the molecular internal energy is increased, the molecular motion rate is increased, the volatilization of low-boiling-point components, such as hydrogen sulfide, acetaldehyde and the like, can be accelerated by the synergistic effect of the two components, so that the white wine can escape out of the wine, and finally the white wine with stable quality can be produced in a short time, so that white wine enterprises can obtain better economic benefit on the premise of ensuring the product quality.
The invention relates to a white spirit metabolic flux analysis method based on ultrasonic wave and ultraviolet light synergistic ripening, which is implemented by using UPC2The QTOF/MS is combined with the metabolic flux analysis method, is used as an effective means system for analyzing a complex system, comprehensively analyzes the material change in a liquor sample system under different ultrasonic wave and ultraviolet light synergistic ripening conditions, explores the white liquor ripening acceleration mechanism of the technology, and provides a theoretical basis for the application of the ultrasonic wave and ultraviolet light synergistic ripening white liquor technology and the metabolic flux analysis method in the field of white liquor production.
Drawings
FIG. 1 is a chart showing the effect of different ultrasonic power conditions on the change of the compound content under the synergistic effect of ultraviolet light;
FIG. 2 is a chart showing the effect of different storage times on the change in compound content after ripening treatment.
Detailed Description
The principles and advantages of the present invention are explained and illustrated below with reference to specific embodiments so that those skilled in the art may better understand the present invention. The following description is exemplary only, and is not intended to limit the scope thereof.
The apparatus used in the invention comprises:
ultra-high performance phase-coincidence chromatography-quadrupole-rod-series time-of-flight mass spectrometer (UPC)2QTOF/MS) (Waters, USA), MS3 vortex apparatus (IKA, Germany), BCD-193MT refrigerator (Kangjia co-generation electric apparatus, Inc., Anhui), PURELA Ultra MK2 Ultra pure water apparatus (ELGA, England), YM-ZCW-1000W microwave, ultrasonic, ultraviolet light catalytic synthesizer (Shanghai Yuming apparatus, Inc.).
The reagent of the invention comprises:
acetonitrile and methanol (Fisher corporation, USA, chromatographic purity); CO 22(purity not less than 99.99%, Shanghai Zhengxing Gauss gas Co., Ltd.); and (3) preparing 9 groups of 6 parallel samples in each group, wherein 1 group is untreated, and respectively carrying out ripening treatment on the other 8 groups under 8 different ultrasonic conditions.
Efficient separation is the key for accurately identifying the components of the liquor system. The diffusion coefficient and viscosity of Supercritical Fluid Chromatography (SFC) are close to those of gas chromatography, so that the mass transfer resistance of solute is small, fast and efficient separation can be obtained, the density of the solute is similar to that of liquid chromatography, and the separation and analysis of thermally unstable substances are facilitated at lower temperature. Ultra-high performance compatible Chromatography (UltraPerformance Convergence Chromatography, abbreviated UPC, in England2) Is a novel chromatographic technique developed based on the basic principle of Supercritical Fluid Chromatography (SFC), can further improve the sensitivity of the method after being combined with mass spectrum, has the advantages of high automation degree, wide application range, strong separation capability, reliable detection result, low detection limit, high analysis speed and the like, and is suitable for the inner group of a liquor system after ripening treatmentScreening and identifying the sub-materials.
The metabolic flux research method adopts a non-targeting method as a research starting point for a specific complex system, and all components are subjected to unbiased detection. And then constructing a corresponding non-targeted analysis model by a multivariate dimension-reducing statistical method, screening out a characteristic compound with group difference, and characterizing the characteristic compound. Can be effectively used for identifying the variety and quality, the origin tracing of the production area, the biological activity, the quality safety of food, the nutrition control and the like of the sample. Therefore, the method is suitable for screening and identifying the component substances in the liquor system after ripening treatment; the ultra-high performance combined chromatography-mass spectrometry technology can effectively make up for the defects of the gas chromatography-mass spectrometry technology in the aspects of substance detection with large polarity, high boiling point and poor thermal stability. And has the advantages of high automation degree, wide application range, strong separation capability, reliable detection result, low detection limit, high analysis speed and the like. Compared with high performance liquid chromatography, the column efficiency of the ultra-high performance combined phase chromatography is about three times that of the high performance liquid chromatography, and the separation time can be effectively shortened. UPC based on the above analysis2The QTOF/MS is suitable for screening and identifying component substances in the white spirit matrix background.
The invention relates to white spirit ripening under the cooperation of ultrasonic waves and ultraviolet light and a metabolic flux analysis method of the white spirit, which comprises the following steps of:
step 1, carrying out ultrasonic wave and ultraviolet light synergistic ripening treatment on the new wine;
the method comprises the following specific steps: when the treatment temperature is 25-35 ℃, the fixed ultraviolet wavelength is 350-385nm (provided by a high-pressure mercury lamp), the power is 180-220W, the ultrasonic frequency is 20-30kHz, and the ultrasonic power is as follows: and treating 8 groups for 15-30min under the conditions of 100W, 150W, 200W, 250W, 300W, 350W, 400W and 450W.
Experiments show that the treatment temperature is 35 ℃, the fixed ultraviolet wavelength is 365nm, the power is 200W, the ultrasonic frequency is 25kHz, the treatment is carried out for 20min, and related data are most easily analyzed on the basis of saving cost, so that the data are adopted to obtain liquor after ripening treatment in the specific treatment process;
UPC2-QTOF/MS assay chromatographic conditions: waters Acquity UPC2CSH Fluoro-phenyl chromatography column: (100 mm. times.3.0 mm,1.8 μm); the column temperature is 34-36 ℃; sample introduction amount: 5 mu L of the solution; temperature of the sample pan: 3-5 ℃; mobile phase: supercritical CO2(A) And methanol/acetonitrile (1:1, v/v) (B); elution gradient: the volume proportion of the mobile phase B is linearly increased from 2 percent to 4 percent within 0-1 min; the volume proportion of the mobile phase B is kept to be 4 percent within 1-6 min; the volume proportion of the mobile phase B is linearly increased to 10 percent from 4 percent within 6 to 6.5 min; the volume proportion of the mobile phase B is kept to be 10 percent within 6.5-14.5 min; the volume proportion of the mobile phase B is linearly reduced to 2 percent from 10 percent within 14.5-15 min; back pressure: 12.00-14.00 MPa; flow rate: 0.4-0.6 mL/min.
UPC2-QTOF/MS mass spectrometry conditions: an ion source: electrospray ion source (ESI); the scanning mode is as follows: ESI positive ion/ESI negative ion; capillary voltage: 3.0-5.0 kV; taper hole voltage: 35-40V; ion source compensation voltage: 80-85V; ion source temperature: 110-130 ℃; temperature of atomized gas: 450 ℃ and 500 ℃; flow rate of atomizing gas: 750-800L/h; taper hole air flow rate: 45-50L/h; scanning mode: full Scan/MSE；MS1And MS2Scanning range: m/z is 100-.
And 3, carrying out chemometric analysis on the measured data result based on a metabolic flux analysis method.
The data processing of the metabolic flow specifically comprises data extraction, data normalization and scaling processing and database online analysis.
The specific operation is as follows: slave UPC2The raw data files obtained by QTOF/MS are collected by the software MS-DIAL for data processing, and the operation items comprise noise filtering, smooth integration, background drift, peak extraction and peak alignment. Identification of compounds and identification of compounds with ddMS using databases METLIN and MassBank2All compounds of the data were subjected to similarity search and peak tables were generated. Peak Table content includes the Retention Time (RT) of metabolites in a sample (i.e., chromatographic peak retention)Time), m/z (i.e. the exact mass of the ion peak) and MS intensity. The MS intensity comprises fragment ion peak intensity and fragment isotope peak intensity, the scanning range m/z is 100-1500, the signal-to-noise ratio threshold (S/N) of peak detection is set to be 3, and the retention time tolerance and the mass tolerance of peak comparison are respectively set to be 0.2min and 0.01 Da. The data are normalized and scaled, namely Sum normalization and logarithmic transformation are carried out, Excel is used for exporting the data into csv files after pareto scaling, online analysis processing is carried out through Metabioanalysis 4.0, and visualization operation of the data is realized.
And 4, carrying out ultrasonic wave and ultraviolet light synergistic ripening treatment on the white spirit sample, storing the white spirit sample at room temperature in a dark place, and sampling and measuring the white spirit sample every 3 days. Sampling, filtering with 0.22 μm organic phase microporous membrane, and performing ultra-high performance combined chromatography-quadrupole rod tandem time-of-flight mass spectrometer (UPC)2QTOF/MS) to study the influence of storage time on the change of compounds in the new wine after ripening treatment;
the method comprises the following specific steps: according to the experimental result in the step 2, the white spirit sample system changes most severely under the 200W treatment condition, so the white spirit sample under the condition is selected to be sampled and measured once every 3 days. Passing through 0.22 μm organic phase microporous filter membrane, and UPC2QTOF/MS data acquisition, repeat step 3 for data analysis. A total of 5 samples were taken and the data collected were visualized as a heat map of the change in compound content in the white wine system in storage time after treatment.
And 5, carrying out sensory evaluation on the white spirit subjected to ultrasonic wave and ultraviolet light synergistic ripening treatment and stored for 15 days by adopting a sequencing test method, and finding out the optimal treatment condition. As can be seen from FIG. 2, the white spirit samples reached a relatively stable state after 12 days of storage. Therefore, the aged wine samples stored for 15 days were subjected to sensory evaluation.
The method comprises the following specific steps: the wine samples stored for 15 days at room temperature in the dark after ripening treatment were selected for sensory evaluation. The untreated wine and the wine samples of 8 different treatment conditions were numbered CL0 (untreated), CL1(100W), CL2(150W), CL3(200W), CL4(250W), CL5(300W), CL6(350W), CL7(400W) and CL8(450W), respectively. 10 participators are qualified and experienced primary-choice judges, and are numbered from J1 to J10. The appearance characteristics and the degree of preference of the sample are evaluated on a numerical scale according to a preset evaluation standard by a scoring analysis method in a sensory evaluation grading test: extremely bad is 1, very bad is 2, bad is 3, generally is 4, well is 5, very well is 6, and extremely well is 7. And then, conducting analysis of variance (ANOVA) on the sensory evaluation result, ensuring the authenticity and objectivity of data, and finally finding out the optimal processing condition, thereby providing a basis for the application of the ultrasonic wave and ultraviolet light synergistic white spirit ripening method in white spirit production.
Analysis results
1 Effect of ultrasound Power on Compound Change
FIG. 1 is a thermal map of the variation of the content of compounds in a white wine system under different sonication conditions. The right column of the figure shows the ratio of molecular weight to retention time and represents the compound corresponding to table 1. The difference in color of the 3 to-3 bands indicates a change in the concentration of the compound in the sample. The rightmost Class band represents a different sample Class. The difference in color exhibited under the different treatment conditions in the graph indicates the magnitude of the change in the degree of the compound during ripening. As can be seen from FIG. 1, the difference between the first 2 lower powers of CL1-CL2 and the last 6 higher powers of CL3-CL8 on the wine compounds is obvious, which indicates that the white wine sample system changes most severely when the ultrasonic power is 200W under the synergistic ripening acceleration of ultraviolet light. Therefore, the sample group data under these conditions were selected, and 46 compounds with significant changes were obtained with 20 (%) as the intra-group difference coefficient threshold, as shown in table 1.
2 Effect of storage time after ripening on Compound Change
A heatmap of the storage time after treatment to the change of the content of compounds in the liquor system is shown in FIG. 2, wherein the right column data in the heatmap is the ratio of the molecular weight of significant difference substances in the liquor system to the retention time along with the change of the storage time after ripening treatment. The change in the color difference of the 3 to-3 bands indicates the change in the concentration of the compound in the sample. The rightmost Class band represents a different sample Class. The difference in color exhibited over time in the graph indicates the magnitude of the change in the compound during storage. D0 represents the untreated wine sample, and D1-D5 represent the number of samples taken every 3 days, respectively. It can be seen from the figure that the substance reaction in the liquor body still proceeds in a short time after the liquor is subjected to ripening treatment, and the color of the heat map remains basically unchanged after D3, which indicates that the liquor system is in a relatively stable state at 12 days.
3 sensory evaluation
The sensory evaluation results are shown in table 2, and the analysis of variance (ANOVA) results are shown in table 3. As can be seen from Table 3, since FA＝3.870796>F(8，89，0.005)＝1.94,FB＝0.377962<F (9,89,0.005) ═ 2.54, so at a confidence of 0.5%, there was a significant difference between the treated samples and no significant difference between the assessors. The sensory evaluation result can be proved to be effective data. From fig. 2, it can be seen that the quality of the wine treated by ultrasonic wave and ultraviolet light in cooperation with ripening is improved compared with the wine not treated, and the quality is improved along with the increase of the ultrasonic power, and the quality is reduced when the treatment condition reaches a certain degree. The best organoleptic quality of the wine was obtained under CL3 (200W). The organic molecular group absorbs ultraviolet energy, so that the molecular potential energy is increased, the high-energy bond positions among molecules are broken and recombined, and the chemical change process of the wine is greatly accelerated by increasing the rate of the intermolecular oxidation, esterification and condensation self-polymerization chemical reaction. The ultrasonic treatment can enhance the molecular activation of various substances, improve the effective collision rate among molecules, further accelerate the esterification, condensation and oxidation reduction reaction, and is favorable for forming the fragrance of the brewed alcohol ester of the white spirit. Meanwhile, the ultrasonic wave can increase the affinity among polar molecules such as water, alcohol, aldehyde, acid, ester and the like, enhance the association degree of ethanol and water molecules, form large and firm polar molecule association groups, reduce the stimulation of the polar molecule association groups on taste organs and ensure that the wine body gradually becomes soft from burst hot. In addition, the ultrasonic can increase the molecular kinetic energy, and when the ultraviolet frequency is consistent with the stretching vibration frequency which can characterize the characteristic group frequency in the group (C-H, O-H, C-O, C ═ O) of the functional group of the main components of the wine such as aldehyde, alcohol, acid, ester, etc., resonance absorption can occur, and the characterized energy can excite the organic molecules to generate strong vibration and rotation, increase the molecular internal energy and increase the molecular motion rate, andthe synergistic effect of the above components can accelerate the volatilization of low boiling point components such as hydrogen sulfide and acetaldehyde, so that the low boiling point components can escape out of the wine. And the excessively high ultrasonic power enables polar molecule association groups originally formed in the wine body to be broken up, and volatile flavor substances to largely escape from a white wine system, so that the quality of the white wine is sharply reduced.
TABLE 1 differential Compounds before and after ripening
TABLE 2 sensory evaluation results
TABLE 3 ANOVA TABLE
Claims (9)
1. A method for accelerating the ripening of white spirit based on ultrasonic wave and ultraviolet light is characterized in that the white spirit after the ripening treatment is obtained by simultaneously carrying out ultraviolet light and ultrasonic wave treatment on new white spirit under the following conditions;
the wavelength of the ultraviolet light is 350-385nm, and the power is 180-220W; the frequency of the ultrasonic wave is 20-30kHz, and the power is 100-450W.
2. The method for accelerating the ripening of white spirit based on the combination of ultrasonic waves and ultraviolet light according to claim 1, wherein the new wine is subjected to both ultraviolet light and ultrasonic treatment at 25-35 ℃.
3. The method for accelerating the ripening of the white spirit based on the combination of the ultrasonic waves and the ultraviolet light according to claim 1, wherein the ultraviolet light and the ultrasonic waves are simultaneously performed on the new white spirit for 15-30 min.
4. The method for accelerating the ripening of the white spirit based on the combination of the ultrasonic waves and the ultraviolet light according to claim 1, wherein the fresh white spirit is subjected to the ultraviolet light and the ultrasonic wave simultaneously under the conditions and then is stored at room temperature in a dark place for at least 15 days.
5. White spirit obtained by the method for ripening white spirit based on ultrasonic wave in cooperation with ultraviolet light according to any one of claims 1 to 4.
6. A method for analyzing metabolic flux of white spirit based on ultrasonic wave and ultraviolet light synergistic ripening is characterized by comprising the following steps:
step 1, filtering the white spirit according to claim 5 by using an organic phase microporous filter membrane, and performing data acquisition by adopting ultra-high performance phase combination chromatography-quadrupole time-of-flight mass spectrometry to obtain an original data file, wherein the conditions of the chromatography and the mass spectrometry are as follows;
the chromatographic column is Waters Acquity UPC2CSH Fluoro-phenyl with column temperature of 34-36 deg.C, sample plate temperature of 3-5 deg.C, and supercritical CO as mobile phase A2The mobile phase B is a mixed solution of methanol and acetonitrile, the volume ratio of the methanol to the acetonitrile is 1:1, the back pressure is 12.00-14.00MPa, and the flow rate is 0.4-0.6 mL/min;
the ion source is an electrospray ion source, the capillary voltage is 3.0-5.0kV, the taper hole voltage is 35-40V, the ion source compensation voltage is 80-85V, and the ion source temperature is 110-130 ℃; the temperature of the atomizing gas is 450-500 ℃, the airflow speed of the atomizing gas is 750-800L/h, and the airflow speed of the taper hole is 45-50L/h;
step 2, extracting the original data file collected in the step 1 and generating a peak table;
and 3, normalizing and scaling the retention time of the metabolites in the peak table, the accurate mass of the ion peak, the fragment ion peak intensity and the fragment isotope peak intensity, and then exporting to obtain a csv file, and performing visual operation on the csv file to finish the analysis of the metabolic flux of the white spirit based on ultrasonic wave and ultraviolet light synergistic ripening.
7. The method for analyzing the metabolic flux of the white spirit based on the ultrasonic wave and ultraviolet light synergistic ripening, according to claim 6, wherein in the step 1, the mobile phase A and the mobile phase B are performed in a gradient elution mode: the volume proportion of the mobile phase B is linearly increased from 2 percent to 4 percent within 0-1 min; the volume proportion of the mobile phase B is kept to be 4 percent within 1-6 min; the volume proportion of the mobile phase B is linearly increased to 10 percent from 4 percent within 6 to 6.5 min; the volume proportion of the mobile phase B is kept to be 10 percent within 6.5-14.5 min; the volume proportion of the mobile phase B is linearly reduced from 10 percent to 2 percent within 14.5-15 min.
8. The method for analyzing the metabolic flux of white spirit based on ultrasonic wave and ultraviolet light synergistic ripening, as claimed in claim 6, wherein in step 1, the scanning mode of mass spectrum is ESI positive ions/ESI negative ions, and the scanning mode is Full Scan/MSE，MS1And MS2The scanning range is m/z is 100-.
9. The method for analyzing metabolic flux of white spirit based on ultrasonic wave and ultraviolet light accelerated ripening of claim 6, wherein step 2 is to perform noise filtering, smooth integration, background drift, peak extraction and peak alignment on the original data file, then identify the compound and perform ddMS on the compound2All compounds of the data were subjected to a similarity search, generating a peak table.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011017253.1A CN112175779B (en) | 2020-09-24 | 2020-09-24 | White spirit ripening based on ultrasonic wave and ultraviolet light cooperation and ripening method and metabolic flow analysis method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202011017253.1A CN112175779B (en) | 2020-09-24 | 2020-09-24 | White spirit ripening based on ultrasonic wave and ultraviolet light cooperation and ripening method and metabolic flow analysis method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN112175779A true CN112175779A (en) | 2021-01-05 |
| CN112175779B CN112175779B (en) | 2023-04-28 |
Family
ID=73955558
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202011017253.1A Active CN112175779B (en) | 2020-09-24 | 2020-09-24 | White spirit ripening based on ultrasonic wave and ultraviolet light cooperation and ripening method and metabolic flow analysis method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN112175779B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113624862A (en) * | 2021-07-13 | 2021-11-09 | 清华大学 | Metabolome covering multiple metabolites, metabolic flux analysis method and kit |
| CN118427541A (en) * | 2024-07-05 | 2024-08-02 | 青岛和微电子有限公司 | Control method, device, equipment and storage medium for wine ripening process parameters |
Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2213729Y (en) * | 1994-10-19 | 1995-11-29 | 顾成全 | Intelligence self-flow type wine composition catalyze equipment |
| CN104560587A (en) * | 2014-12-10 | 2015-04-29 | 惠州学院 | Method for promoting aging of fruit-type white spirit under actions of infrared assisted ultrasonic and pulse electric field |
| CN105572249A (en) * | 2015-12-15 | 2016-05-11 | 宜宾五粮液股份有限公司 | Method for carrying out risk assessment on influence of activated carbon on wine product |
| CN106367279A (en) * | 2016-08-30 | 2017-02-01 | 惠州学院 | Processing method for enhancing aroma of fruit baijiu |
| CN106404956A (en) * | 2016-09-30 | 2017-02-15 | 山东省分析测试中心 | Method for detecting four organic acids in wine and/or fruit wine at same time through high performance liquid chromatography-tandem mass spectrometry internal standard method and application of method |
| CN106442766A (en) * | 2016-08-31 | 2017-02-22 | 安徽瑞思威尔科技有限公司 | Method for fast detecting gamma-aminobutyric acid in baijiu |
| CN106483241A (en) * | 2016-10-28 | 2017-03-08 | 陕西科技大学 | The Ultra Performance Liquid Chromatography level Four bar electrostatic field orbit ion trap mass spectrum screening method of pigment in wine |
| CN106596792A (en) * | 2016-12-30 | 2017-04-26 | 四川剑南春（集团）有限责任公司 | Method for detecting content of aromatic ester substances in Baijiu |
| CN108535395A (en) * | 2018-03-12 | 2018-09-14 | 安徽古井贡酒股份有限公司 | A method of using 32 kinds of free fatties in UPLC-QTof Rapid Simultaneous Determination health liquors |
| CN109517712A (en) * | 2018-12-25 | 2019-03-26 | 周相真 | A kind of method and apparatus of new wine accelerated ageing |
| JP2019070548A (en) * | 2017-10-06 | 2019-05-09 | 独立行政法人酒類総合研究所 | Method for preparing prediction formula for predicting brewing characteristics of brewing raw material grain, and method for producing grain varieties using prediction formula |
| CN109828045A (en) * | 2019-02-21 | 2019-05-31 | 安徽古井贡酒股份有限公司 | A kind of method that ultra high efficiency closes 13 kinds of isoflavones in phase chromatography concatenation QDa while quickly detection alcohol product |
| CN109828044A (en) * | 2019-02-21 | 2019-05-31 | 安徽古井贡酒股份有限公司 | A kind of method that ultra high efficiency closes 8 kinds of phenolic acids in phase chromatography concatenation QDa while quickly detection alcohol product |
| CN110954610A (en) * | 2019-11-15 | 2020-04-03 | 陕西西凤酒股份有限公司 | Method for simultaneously detecting six sweetening agents in Feng-flavor liquor by high performance liquid chromatography-mass spectrometry |
-
2020
- 2020-09-24 CN CN202011017253.1A patent/CN112175779B/en active Active
Patent Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2213729Y (en) * | 1994-10-19 | 1995-11-29 | 顾成全 | Intelligence self-flow type wine composition catalyze equipment |
| CN104560587A (en) * | 2014-12-10 | 2015-04-29 | 惠州学院 | Method for promoting aging of fruit-type white spirit under actions of infrared assisted ultrasonic and pulse electric field |
| CN105572249A (en) * | 2015-12-15 | 2016-05-11 | 宜宾五粮液股份有限公司 | Method for carrying out risk assessment on influence of activated carbon on wine product |
| CN106367279A (en) * | 2016-08-30 | 2017-02-01 | 惠州学院 | Processing method for enhancing aroma of fruit baijiu |
| CN106442766A (en) * | 2016-08-31 | 2017-02-22 | 安徽瑞思威尔科技有限公司 | Method for fast detecting gamma-aminobutyric acid in baijiu |
| CN106404956A (en) * | 2016-09-30 | 2017-02-15 | 山东省分析测试中心 | Method for detecting four organic acids in wine and/or fruit wine at same time through high performance liquid chromatography-tandem mass spectrometry internal standard method and application of method |
| CN106483241A (en) * | 2016-10-28 | 2017-03-08 | 陕西科技大学 | The Ultra Performance Liquid Chromatography level Four bar electrostatic field orbit ion trap mass spectrum screening method of pigment in wine |
| CN106596792A (en) * | 2016-12-30 | 2017-04-26 | 四川剑南春（集团）有限责任公司 | Method for detecting content of aromatic ester substances in Baijiu |
| JP2019070548A (en) * | 2017-10-06 | 2019-05-09 | 独立行政法人酒類総合研究所 | Method for preparing prediction formula for predicting brewing characteristics of brewing raw material grain, and method for producing grain varieties using prediction formula |
| CN108535395A (en) * | 2018-03-12 | 2018-09-14 | 安徽古井贡酒股份有限公司 | A method of using 32 kinds of free fatties in UPLC-QTof Rapid Simultaneous Determination health liquors |
| CN109517712A (en) * | 2018-12-25 | 2019-03-26 | 周相真 | A kind of method and apparatus of new wine accelerated ageing |
| CN109828045A (en) * | 2019-02-21 | 2019-05-31 | 安徽古井贡酒股份有限公司 | A kind of method that ultra high efficiency closes 13 kinds of isoflavones in phase chromatography concatenation QDa while quickly detection alcohol product |
| CN109828044A (en) * | 2019-02-21 | 2019-05-31 | 安徽古井贡酒股份有限公司 | A kind of method that ultra high efficiency closes 8 kinds of phenolic acids in phase chromatography concatenation QDa while quickly detection alcohol product |
| CN110954610A (en) * | 2019-11-15 | 2020-04-03 | 陕西西凤酒股份有限公司 | Method for simultaneously detecting six sweetening agents in Feng-flavor liquor by high performance liquid chromatography-mass spectrometry |
Non-Patent Citations (3)
| Title |
|---|
| 朱文星 等: "超高效合相色谱串联四级杆飞行时间质谱定性分析中/长链结构甘油三酯组成", 《中国药学杂志》 * |
| 李大和 等: "《浓香型曲酒生产技术》", 31 March 1994 * |
| 程明川 等: "基于高分辨质谱和代谢组学分析方法的白酒成分分析和香型鉴别", 《环境化学》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113624862A (en) * | 2021-07-13 | 2021-11-09 | 清华大学 | Metabolome covering multiple metabolites, metabolic flux analysis method and kit |
| CN118427541A (en) * | 2024-07-05 | 2024-08-02 | 青岛和微电子有限公司 | Control method, device, equipment and storage medium for wine ripening process parameters |
Also Published As
| Publication number | Publication date |
|---|---|
| CN112175779B (en) | 2023-04-28 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN112175779A (en) | White spirit based on ultrasonic wave and ultraviolet light synergistic ripening acceleration and ripening acceleration method and metabolic flux analysis method thereof | |
| Xiao et al. | Characterization of different aroma‐types of chinese liquors based on their aroma profile by gas chromatography–mass spectrometry and sensory evaluation | |
| Španěl et al. | Reactions of H3O+ and OH− ions with some organic molecules; applications to trace gas analysis in air | |
| Ma et al. | Variations in physicochemical properties of Chinese Fenjiu during storage and high-gravity technology of liquor aging | |
| Smith et al. | Reactions of the selected ion flow tube mass spectrometry reagent ions H3O+ and NO+ with a series of volatile aldehydes of biogenic significance | |
| Taylor et al. | Non-destructive and high-throughput—APCI-MS, PTR-MS and SIFT-MS as methods of choice for exploring flavor release | |
| CN108845067B (en) | Purging and trapping method for flavor components in tobacco and tobacco products | |
| Zhou et al. | Coupling neutral desorption sampling to dielectric barrier discharge ionization mass spectrometry for direct oil analysis | |
| Shi et al. | Rapid screening of illegally added drugs in functional food using a miniature ion trap mass spectrometer | |
| CN109459484A (en) | A kind of mass spectrometric analysis method of the small molecule sample based on nano material | |
| Xiang et al. | Development of electrospray/photoionization miniature ion trap mass spectrometer | |
| Black et al. | Determination of metal chelates by inductively coupled plasma atomic emission spectrometry and applications to biological materials | |
| JP2016057220A (en) | Analysis method of lipid | |
| Licen et al. | Derivatized volatile organic compound characterization of Friulano wine from Collio (Italy–Slovenia) by HS-SPME-GC-MS and discrimination from other varieties by chemometrics | |
| CN115950979A (en) | Method for tracing origin of complex matrix tobacco extract | |
| CN114924002A (en) | Method for identifying NFC and FC orange juice by combining metabonomics technology and machine learning | |
| Janda et al. | Study of plasma induced chemistry by DC discharges in CO2/N2/H2O mixtures above a water surface | |
| CN112530527A (en) | Method for establishing molecular network based on GC-MS and application thereof | |
| CN111426742A (en) | Application of silver nanowire material as MA L DI-TOF MS matrix in metabolite detection | |
| Wang et al. | Development of a flavor fingerprint by gas chromatography ion mobility spectrometry with principal component analysis for volatile compounds from Eucommia ulmoides Oliv. leaves and its fermentation products | |
| CN115825308B (en) | Application of nasopharyngeal carcinoma related urine marker in preparation of product for diagnosing/prognosing nasopharyngeal carcinoma | |
| CN110672708A (en) | Ethylene detection method based on ion mobility spectrometry technology | |
| CN114216835B (en) | Method for screening biological metabolism marker of seaweed polysaccharide colon cancer resistance activity and application | |
| Schacker et al. | Study of viability of solid-phase microextraction, in vivo, in the extraction of microbial volatile organic compounds associated to the pigment production process by the Monascus fungus, in submerged fermentation | |
| Pinu | Sauvignon blanc metabolomics: Metabolite profile analysis before and after fermentation |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |