Development method of special liqueur product based on flavor orientation

Abstract

The invention discloses a special liqueur product development method based on flavor guidance, which comprises the following steps: determining a special liqueur formula medicine flavor, and trial-producing a special liqueur sample; sensory flavors of different characteristic liqueur samples are analyzed through sensory evaluation, flavor substances and component flavor substances of the characteristic liqueur samples and aroma contributions of the flavor substances are analyzed, the content of the flavor substances in the characteristic liqueur samples is determined, and the range of the content of the flavor substances represented by sensory attributes is determined by combining a flavor fusion result. On the basis of sensory omics and flavor omics, consumer preference is taken as a guide, sensory evaluation and instrumental analysis of the liqueur are integrated, important sensory characteristic substances of the liqueur are determined while effective components of medicinal flavors of a liqueur formula are ensured, so that the flavor of the base wine and the flavor of a raw material formula are fully fused, and the flavor of the liqueur is improved. The method solves the problems that the aroma of the wine body is not pure enough and not mellow enough, and the like, can objectively, scientifically and accurately evaluate the flavor adaptability of the base wine and the formula, improves the drinking palatability and pleasure, and promotes the improvement of the industry quality.

Description

Technical Field

[0001] The invention belongs to the technical field of liquor product development, and in particular relates to a flavor-guided characteristic liquor product development method. Background Art

[0002] Lujiu is a beverage alcoholic beverage with a specific style, made from yellow wine or white wine, with the addition of materials that are traditionally both food and Chinese medicinal materials or specific food raw materials or materials that comply with relevant regulations, through extraction and (or) double distillation or directly adding specific ingredients extracted from food, without directly or indirectly adding food additives. Lujiu, as an important category of beverage alcoholic beverages, not only has a unique flavor and color, but also retains the medicinal effects of the medicinal taste of medicine and food. Compared with distilled alcoholic beverages brewed from grains, it has higher nutritional content and flavor. At present, the production process of Lujiu in enterprises generally adopts the method of soaking raw materials in white wine to obtain the extract, and then dilutes and reduces the degree of the extract as the original wine of Lujiu. Such a production process not only dilutes the effective ingredients of the Lujiu extract, but also destroys the original flavor of Lujiu, making it difficult to integrate the flavor of the base wine with the flavor of the formula, resulting in the disharmony and roundness of the aroma of the Lujiu. Flavor and functional attributes directly affect consumers' acceptance of wine products. Unclear wine flavor characteristics will directly lead to a gap between product flavor characteristics and consumer matching, thus hindering the development of the wine industry. However, current research on wine focuses on production technology and processing methods, and lacks research on wine flavor. How to ensure that wine has a distinctive flavor, good drinking palatability and pleasure while maintaining the style of wine products as both medicine and food is a major problem in the development of wine products. Summary of the invention

[0003] The purpose of the present invention is to provide a method for developing a special liquor product based on flavor orientation, which integrates expert liquor sensory evaluation and professional instrument analysis to objectively, scientifically and accurately evaluate the flavor compatibility of base liquor and formula, and develop a liquor product with a unique style.

[0004] The technical solution of the present invention is: a method for developing a flavor-oriented special liquor product, comprising the following steps:

[0005] A: Determine the medicinal flavor of the special wine formula;

[0006] B: Using liquor as the base liquor, directly soaking a certain amount of the formula, trial-producing special liquor samples, and analyzing the sensory flavors of different special liquor samples through sensory evaluation;

[0007] B1: Invite 5 national-level wine judges to form an expert panel;

[0008] B2: Five expert tasters conducted sensory evaluation on the appearance and color (20 points), aroma (30 points), taste and texture (40 points), and style (10 points) of the wine. The average score of the expert tasters was used as the comprehensive sensory evaluation score of the featured wine samples.

[0009] B3: According to the scoring results, the sensory evaluation comprehensive score of the characteristic wine sample is greater than 90 points, which is determined as a good level of wine flavor adaptability; the sensory evaluation comprehensive score of the characteristic wine sample is 80-90 points, which is determined as a general level of wine flavor adaptability; the sensory evaluation comprehensive score of the characteristic wine sample is less than 80 points, which is determined as a poor level of wine flavor adaptability;

[0010] C: Comprehensively adopt olfactory and gas chromatography-mass spectrometry analysis technology to analyze the flavor substances of the special wine samples and clarify the flavor substances of the special wine samples and their aroma contribution;

[0011] C1: Select 7890A-5975C gas chromatograph-mass spectrometer and DB-FFAP capillary column (30m×0.25mm, 0.25μm); select characteristic liquor samples with a comprehensive sensory evaluation score of >90 points;

[0012] C2: Measure 1 mL of the specialty wine sample into a 10 mL screw-thread bottle, add 9.6 mL of saturated sodium chloride solution, and store at 4 °C for testing;

[0013] C3: Set up 7890A-5975C gas chromatograph-mass spectrometer and DB-FFAP capillary column (30m×0.25mm, 0.25μm); the injection port temperature is 250℃, the carrier gas is helium, the flow rate is 1mL / min, non-split injection, and the temperature is programmed; 40℃ is maintained for 1min, 3℃ / min is increased to 130℃ and maintained for 0min, 10℃ / min is increased to 220℃ and maintained for 10min; mass spectrometry conditions: EI ion source, electron energy is 70eV, ion source temperature is 230℃, quadrupole temperature is 150℃, solvent delay is 0min, acquisition mode is SIM / Scan, and the scanning range is m / z 35~550amu;

[0014] C4: Select 3 professional researchers in the field of liquor flavor and quality to form a sniffing panel. The sniffing panel members sniff at the sniffing port and record the retention time, aroma description and aroma intensity of the sensory attribute characteristic compounds at the same time; each person sniffs the same sample 3 times, and the aroma intensity is evaluated using a three-point method of 0 to 3 points: "0" means no aroma, "1" means weak aroma intensity, "2" means medium aroma intensity, and "3" means strong aroma intensity; the compounds smelled by all three sniffing panel members, with similar sensory descriptions and the average aroma intensity are taken as the analysis results;

[0015] D: Comprehensively use olfaction and gas chromatography-mass spectrometry analysis technology to analyze the flavor substances in the special wine formula and clarify the flavor substances in the formula and their aroma contribution;

[0016] D1: After grinding the ingredients of the formula, weigh 2g of the ingredients of the formula into a 20mL headspace screw bottle and store at 4℃ for testing;

[0017] D2: Set up 7890A-5975C gas chromatograph-mass spectrometer and DB-FFAP capillary column (30m×0.25mm, 0.25μm); the injection port temperature is 250℃, the carrier gas is helium, the flow rate is 1mL / min, non-split injection, and the temperature is programmed; 40℃ is maintained for 1min, 3℃ / min is increased to 130℃ and maintained for 0min, 10℃ / min is increased to 220℃ and maintained for 10min; mass spectrometry conditions: EI ion source, electron energy is 70eV, ion source temperature is 230℃, quadrupole temperature is 150℃, solvent delay is 0min, acquisition mode is SIM / Scan, and the scanning range is m / z 35~550amu;

[0018] D3: Three professional researchers in the field of liquor flavor and quality were selected to form a sniffing panel. The sniffing panel members sniffed at the sniffing port and recorded the retention time, aroma description and aroma intensity of the sensory attribute characteristic compounds at the same time; each person sniffed the same sample three times, and the aroma intensity was evaluated using a three-point method of 0 to 3 points: "0" means no aroma, "1" means weak aroma intensity, "2" means medium aroma intensity, and "3" means strong aroma intensity; the compounds smelled by all three sniffing panel members, with similar sensory descriptions and the average aroma intensity were taken as the analysis results;

[0019] E: Establish a quantitative analysis method for flavor substances in special wine samples to determine the content of flavor substances in special wine samples;

[0020] E1: Select samples, standards, and reagents

[0021] Sample: Specialty wine samples

[0022] Standards: acetic acid, propionic acid, butyric acid, 3-methylbutyric acid, isobutyric acid, ethyl phenylacetate, phenylethyl acetate, ethyl 3-phenylpropionate, acetophenone, phenylethanol, ethyl butyrate, ethyl 2-methylbutyrate, ethyl valerate, ethyl octanoate, ethyl lactate, ethyl benzoate, γ-nonalactone, trimethylpyrazine, furfural, 2-acetylfuran, (±)-limonene, α-cedrene, α-cedrol, hexanal, benzaldehyde, citronellol;

[0023] Reagents: n-butanol (analytical grade), ether (analytical grade), ethanol (analytical grade), n-pentane (chromatographic grade), dichloromethane (chromatographic grade), n-hexane (chromatographic grade), ethyl acetate (chromatographic grade);

[0024] E2: Select instruments and equipment

[0025] A 7890A-5975C gas chromatograph-mass spectrometer, an HP-5 capillary column (30 m × 0.25 mm, 0.25 μm), a DB-WAX UI capillary column (30 m × 0.25 mm, 0.25 μm), a DB-FFAP capillary column (30 m × 0.25 mm, 0.25 μm), a DB-5MS capillary column (30 m × 0.25 mm, 0.25 μm), a Mikro220R centrifuge, a VORTEX-GENIE adjustable speed timing vortex mixer, an MS1602TS electronic balance, and a Branson3210 ultrasonic cleaner were used.

[0026] E3: Measure 5 mL of the specialty liquor sample into a 50 mL centrifuge tube with a scale, add 20 mL of saturated sodium chloride aqueous solution, 2 μL of 11727 mg / L citronellol internal standard, use 2 mL of ethyl acetate, vortex for 1 min, centrifuge and extract, take the upper organic phase, and store it at 4 °C for testing;

[0027] E4: Chromatographic conditions: Column: HP-5 capillary column (30m×0.25mm, 0.25μm), DB-FFAP capillary column (30m×0.25mm, 0.25μm), DB-WAX UI capillary column (30m×0.25mm, 0.25μm); Temperature program: 40℃ for 1min, 5℃ / min to 230℃ for 10min; Injection port temperature 250℃, carrier gas helium, flow rate 1.0mL / min, splitless injection, injection volume 1μL;

[0028] E5: Mass spectrometry conditions: electron impact ionization source, electron energy of 70 eV, ion source temperature of 230 °C, quadrupole temperature of 150 °C; solvent delay: 5.0 min, acquisition mode of full scan, scanning range of m / z 35-350 amu;

[0029] E6: Qualitative and quantitative analysis

[0030] The retention index of the compound was qualitatively determined by comparing it with the NIST14 spectral library and standard verification;

[0031] A certain concentration of flavor substance standard solution was prepared with 53% ethanol solution, 5 mL of the standard solution was measured and placed in a 50 mL centrifuge tube with a scale, 20 mL of saturated sodium chloride aqueous solution and 2 μL of citronellol internal standard with a concentration of 11727 mg / L were added, 2 mL of ethyl acetate was used, vortexed for 1 min, centrifuged and extracted, the upper organic phase was taken, and stored at 4°C for testing; a standard curve was established by the mass concentration of the standard sample / internal standard concentration-peak area of ​​the standard solution / peak area of ​​the internal standard; the mass concentration with a chromatographic peak signal-to-noise ratio greater than 3 was determined as the detection limit, and the mass concentration with a signal-to-noise ratio greater than 10 was determined as the quantification limit;

[0032] E7: Results and Optimization

[0033] E71: Sample preparation optimization

[0034] Alcohol content dilution of characteristic liquor: 5 mL of liquor sample was measured and put into a white sample bottle, and different volumes of saturated sodium chloride aqueous solution were added respectively, and the alcohol content of the characteristic liquor sample was diluted to 12% vol, 10% vol, 9% vol, 8% vol, 7% vol, and 6% vol, and 2 μL of citronellol internal standard with a concentration of 11727 mg / L and 2 mL of ethyl acetate were added respectively, and the mixture was vortexed for 1 min, and the upper organic phase was centrifuged to be tested, and the extraction effect of the same extraction solvent on the characteristic liquor flavor substances at different alcohol content was compared; the total peak area and the total peak number of the flavor substances of the characteristic liquor sample were used as the measurement indicators, and the alcohol content of 10% vol when the total peak area and the total peak number of the flavor substances of the characteristic liquor sample were both high and the extraction effect of the flavor substances of the characteristic liquor sample was the best was found as the optimal analytical alcohol content;

[0035] Selection of extraction solvents for specialty liquor samples: Different solvents have different extraction efficiencies for flavor substances in specialty liquor samples. Under the optimal analytical alcohol content and other constant conditions, the extraction effects of ethyl acetate, ether, n-hexane, n-butanol, n-pentane, dichloromethane and other solvents on flavor substances in the same specialty liquor sample were compared. Taking the total peak area and total peak number of liquor flavor substances as measurement indicators, ethyl acetate, which has the largest total number of extracted peaks and the highest total peak area, was selected as the optimal extraction solvent.

[0036] Optimization of the amount of extraction solvent: Under other constant conditions, the effect of the solid-liquid ratio on the extraction effect was investigated. The extraction of flavor substances in the same special wine sample was analyzed when the solid-liquid ratio was 5:1, 5:2, 5:3, 5:4, 5:5, and 5:10. 2 mL of extraction solvent was selected as the optimal amount of extractant, that is, the solid-liquid ratio was 5:2;

[0037] E72: Optimization of instrumental analysis methods

[0038] Instrumental chromatographic column optimization: DB-WAX-UI capillary column, DB-FFAP capillary column, and HP-5 capillary column were compared. The column parameters were all 30m×0.25mm×0.25μm. The total peak area and total peak number of the flavor substances in the wine samples were used as the measurement indicators for the analysis effect. The DB-WAX-UI capillary column with the largest number of extracted flavor substances was selected as the best gas phase capillary column.

[0039] E73: Flavor substance information and spiked recovery of specialty liquor samples

[0040] The same sensory attribute flavor of the characteristic liquor samples is contributed by the flavor substances with similar sensory characteristics in the formula and the liquor. The flavor substances with similar sensory characteristics are clustered and quantitatively analyzed as follows: a certain concentration gradient of flavor substances is prepared in ethyl acetate solution, 2 μL of citronellol with a concentration of 11727 mg / L is added as the internal standard, the ratio of the peak area of ​​citronellol to the peak area of ​​the internal standard is used as the ordinate, and the concentration ratio is used as the abscissa to draw a standard curve, and the signal-to-noise ratio is used as the standard to calculate the detection limit LOD and the quantification limit LOQ of the flavor substances under the experimental conditions;

[0041] F: Combined with the flavor fusion results of the specialty liquor samples, determine the content range of flavor substances representing the sensory attributes in the specialty liquor samples.

[0042] F1: Adaptation to different styles of base wine

[0043] Compare and analyze the compatibility of three different styles of base wines with the medicinal flavors of the formula, and determine the best base wine based on the taste and flavor characteristics of the special wine samples. After sensory evaluation by the expert group, select the base wine used by the special wine sample with the largest comprehensive sensory evaluation score as the best base wine;

[0044] F2: Special wine soaking parameters

[0045] The changes in sensory and physical and chemical indices of the characteristic liquor samples were compared and analyzed under different soaking times of 20 days, 30 days, 40 days and 50 days, and different soaking amounts of functional excipients of 0.5%, 1%, 1.5% and 2%. The safe and effective content range of the functional factors reported in the literature was compared. Combined with the sensory evaluation results of the expert group, the optimal soaking process was selected, which was 2% and 40 days, which could extract the functional factors efficiently and quickly without affecting the sensory flavor fusion of the characteristic liquor samples.

[0046] F3: Analyze the content of representative flavor substances of the characteristic liquor samples with the same sensory attributes in the best soaking process samples, and determine the content range of representative flavor substances of the characteristic liquor samples with the sensory attributes in combination with the flavor fusion results of the characteristic liquor samples;

[0047] F4: Combine the sensory evaluation results of the characteristic liquor samples with the content of flavor substances represented by the sensory attributes of the characteristic liquor samples. When the sensory tasting score of the characteristic liquor samples reaches 90 points or above, and the content range of the characteristic flavor represented by the sensory attributes is within the content range of the flavor substances represented by the sensory attributes of the characteristic liquor samples determined in F3, it can be determined that the sensory style characteristics of the characteristic liquor samples are typical, and have good compatibility and integration with the formula.

[0048] The present invention is based on sensory omics and flavor omics, is guided by consumer preferences, integrates sensory evaluation of Lu wine and instrumental analysis, and clarifies important sensory characteristic substances of Lu wine while ensuring the effective ingredients of the medicinal flavor of the Lu wine formula, so that the flavor of the base wine and the flavor of the raw material formula are fully integrated, ensuring that the Lu wine has a distinctive flavor, and solving the problems of the wine aroma being not pure and mellow enough. The present invention can objectively, scientifically and accurately evaluate the flavor compatibility of the base wine and the formula, and can also control the quality of the Lu wine product from the perspective of flavor, thereby improving the drinking palatability and pleasure, and promoting quality improvement in the industry. BRIEF DESCRIPTION OF THE DRAWINGS

[0049] Figure 1 It is a flow chart of the present invention;

[0050] Figure 2 This is a diagram showing the extraction effects of flavor substances in liquors with different alcohol contents;

[0051] Figure 3 Optimize the diagram for extraction solvent;

[0052] Figure 4 Optimization diagram for the amount of extraction solvent;

[0053] Figure 5 Optimize the chart for instrument columns;

[0054] Figure 6 This is the mean value chart of sensory evaluation of samples prepared with different soaking parameters. DETAILED DESCRIPTION

[0055] Embodiment 1: A method for developing a flavor-oriented specialty liquor product, comprising the following steps:

[0056] A: Determine the medicinal flavor of the special wine formula;

[0057] B: Using liquor as the base liquor, directly soak a certain amount of the formula to trial-produce special liquor samples, and analyze the sensory flavors of different special liquor samples through sensory evaluation;

[0058] B1: Invite 5 national-level wine judges to form an expert panel;

[0059] B2: Five expert tasters conducted sensory evaluation on the appearance and color (20 points), aroma (30 points), taste and texture (40 points), and style (10 points) of the wine. The average score of the expert tasters was used as the comprehensive sensory evaluation score of the featured wine samples.

[0060] B3: According to the scoring results, the sensory evaluation comprehensive score of the characteristic wine sample is greater than 90 points, which is determined as a good level of wine flavor adaptability; the sensory evaluation comprehensive score of the characteristic wine sample is 80-90 points, which is determined as a general level of wine flavor adaptability; the sensory evaluation comprehensive score of the characteristic wine sample is less than 80 points, which is determined as a poor level of wine flavor adaptability;

[0061] C: Comprehensively adopt olfactory and gas chromatography-mass spectrometry analysis technology to analyze the flavor substances of the special wine samples and clarify the flavor substances of the special wine samples and their aroma contribution;

[0062] C1: Select 7890A-5975C gas chromatograph-mass spectrometer and DB-FFAP capillary column (30m×0.25mm, 0.25μm); select characteristic liquor samples with a comprehensive sensory evaluation score of >90 points;

[0063] C2: Measure 1 mL of the specialty wine sample into a 10 mL screw-thread bottle, add 9.6 mL of saturated sodium chloride solution, and store at 4 °C for testing;

[0064] C3: Set up 7890A-5975C gas chromatograph-mass spectrometer and DB-FFAP capillary column (30m×0.25mm, 0.25μm); the injection port temperature is 250℃, the carrier gas is helium, the flow rate is 1mL / min, non-split injection, and the temperature is programmed; 40℃ is maintained for 1min, 3℃ / min is increased to 130℃ and maintained for 0min, 10℃ / min is increased to 220℃ and maintained for 10min; mass spectrometry conditions: EI ion source, electron energy is 70eV, ion source temperature is 230℃, quadrupole temperature is 150℃, solvent delay is 0min, acquisition mode is SIM / Scan, and the scanning range is m / z 35~550amu;

[0065] C4: Select 3 professional researchers in the field of liquor flavor and quality to form a sniffing panel. The sniffing panel members sniff at the sniffing port and record the retention time, aroma description and aroma intensity of the sensory attribute characteristic compounds at the same time; each person sniffs the same sample 3 times, and the aroma intensity is evaluated using a three-point method of 0 to 3 points: "0" means no aroma, "1" means weak aroma intensity, "2" means medium aroma intensity, and "3" means strong aroma intensity; the compounds smelled by all three sniffing panel members, with similar sensory descriptions and the average aroma intensity are taken as the analysis results;

[0066] The three members of the olfactory panel smelled 26 compounds that contributed to the aroma in the wine samples. The corresponding compounds and aroma intensity of each aroma are shown in Table 1:

[0067] Table 1 Analysis results of flavor components of liquor

[0068]

[0069] Note: The compounds in the table were identified by mass spectrometry, aroma description, and retention index comparison with that of standards.

[0070] D: Comprehensively use olfaction and gas chromatography-mass spectrometry analysis technology to analyze the flavor substances in the special wine formula and clarify the flavor substances in the formula and their aroma contribution;

[0071] D1: After grinding the ingredients of the formula, weigh 2g of the ingredients of the formula into a 20mL headspace screw bottle and store at 4℃ for testing;

[0072] D2: Set up 7890A-5975C gas chromatograph-mass spectrometer and DB-FFAP capillary column (30m×0.25mm, 0.25μm); the injection port temperature is 250℃, the carrier gas is helium, the flow rate is 1mL / min, non-split injection, and the temperature is programmed; 40℃ is maintained for 1min, 3℃ / min is increased to 130℃ and maintained for 0min, 10℃ / min is increased to 220℃ and maintained for 10min; mass spectrometry conditions: EI ion source, electron energy is 70eV, ion source temperature is 230℃, quadrupole temperature is 150℃, solvent delay is 0min, acquisition mode is SIM / Scan, and the scanning range is m / z 35~550amu;

[0073] D3: Three professional researchers in the field of liquor flavor and quality were selected to form a sniffing panel. The sniffing panel members sniffed at the sniffing port and recorded the retention time, aroma description and aroma intensity of the sensory attribute characteristic compounds at the same time; each person sniffed the same sample three times, and the aroma intensity was evaluated using a three-point method of 0 to 3 points: "0" means no aroma, "1" means weak aroma intensity, "2" means medium aroma intensity, and "3" means strong aroma intensity; the compounds smelled by all three sniffing panel members, with similar sensory descriptions and the average aroma intensity were taken as the analysis results;

[0074] The three members of the olfactory panel smelled 11 compounds that contributed to the aroma in the formula medicinal samples. The corresponding compounds and aroma intensity of each aroma are shown in Table 2.

[0075] Table 2 Analysis results of the flavor components of the prescription

[0076]

[0077] Note: The compounds in the table were identified by mass spectrometry, aroma description, and retention index comparison with that of standards.

[0078] E: Establish a quantitative analysis method for flavor substances in special wine samples to determine the content of flavor substances in special wine samples;

[0079] E1: Select samples, standards, and reagents

[0080] Sample: Specialty wine samples

[0081] Standards: acetic acid, propionic acid, butyric acid, 3-methylbutyric acid, isobutyric acid, ethyl phenylacetate, phenylethyl acetate, ethyl 3-phenylpropionate, acetophenone, phenylethanol, ethyl butyrate, ethyl 2-methylbutyrate, ethyl valerate, ethyl octanoate, ethyl lactate, ethyl benzoate, γ-nonalactone, trimethylpyrazine, furfural, 2-acetylfuran, (±)-limonene, α-cedrene, α-cedrol, hexanal, benzaldehyde, citronellol;

[0082] Reagents: n-butanol (analytical grade), ether (analytical grade), ethanol (analytical grade), n-pentane (chromatographic grade), dichloromethane (chromatographic grade), n-hexane (chromatographic grade), ethyl acetate (chromatographic grade);

[0083] E2: Select instruments and equipment

[0084] 7890A-5975C gas chromatograph-mass spectrometer, HP-5 capillary column (30m×0.25mm, 0.25μm), DB-WAX-UI capillary column (30m×0.25mm, 0.25μm), DB-FFAP capillary column (30m×0.25mm, 0.25μm), DB-5MS capillary column (30m×0.25mm, 0.25μm), Mikro220R centrifuge, VORTEX-GENIE adjustable speed timing vortex mixer, MS1602TS electronic balance, Branson3210 ultrasonic cleaner were selected;

[0085] E3: Measure 5 mL of the specialty liquor sample into a 50 mL centrifuge tube with a scale, add 20 mL of saturated sodium chloride aqueous solution, 2 μL of 11727 mg / L citronellol internal standard, use 2 mL of ethyl acetate, vortex for 1 min, centrifuge and extract, take the upper organic phase, and store it at 4 °C for testing;

[0086] E4: Chromatographic conditions: Column: HP-5 capillary column (30m×0.25mm, 0.25μm), DB-FFAP capillary column (30m×0.25mm, 0.25μm), DB-WAX UI capillary column (30m×0.25mm, 0.25μm); Temperature program: 40℃ for 1min, 5℃ / min to 230℃ for 10min; Injection port temperature 250℃, carrier gas helium, flow rate 1.0mL / min, splitless injection, injection volume 1μL;

[0087] E5: Mass spectrometry conditions: electron impact ionization source, electron energy of 70 eV, ion source temperature of 230 °C, quadrupole temperature of 150 °C; solvent delay: 5.0 min, acquisition mode of full scan, scanning range of m / z 35-350 amu;

[0088] E6: Qualitative and quantitative analysis

[0089] The retention index of the compound was qualitatively determined by comparing it with the NIST14 spectral library and standard verification;

[0090] A certain concentration of flavor substance standard solution was prepared with 53% ethanol solution, 5 mL of the standard solution was measured and placed in a 50 mL centrifuge tube with a scale, 20 mL of saturated sodium chloride aqueous solution and 2 μL of citronellol internal standard with a concentration of 11727 mg / L were added, 2 mL of ethyl acetate was used, vortexed for 1 min, centrifuged and extracted, the upper organic phase was taken, and stored at 4°C for testing; a standard curve was established by the mass concentration of the standard sample / internal standard concentration-peak area of ​​the standard solution / peak area of ​​the internal standard; the mass concentration with a chromatographic peak signal-to-noise ratio greater than 3 was determined as the detection limit, and the mass concentration with a signal-to-noise ratio greater than 10 was determined as the quantification limit;

[0091] E7: Results and Optimization

[0092] E71: Sample preparation optimization

[0093] Alcohol content dilution of characteristic liquor: 5 mL of liquor sample was measured and put into a white sample bottle, and different volumes of saturated sodium chloride aqueous solution were added to dilute the alcohol content of the characteristic liquor sample to 12% vol, 10% vol, 9% vol, 8% vol, 7% vol, and 6% vol, and 2 μL of citronellol internal standard with a concentration of 11727 mg / L and 2 mL of ethyl acetate were added respectively. The mixture was vortexed for 1 min, and the upper organic phase was centrifuged to be tested. The extraction effect of the same extraction solvent on the characteristic liquor flavor substances at different alcohol content was compared; the total peak area and the total number of peaks of the flavor substances of the characteristic liquor sample were used as the measurement indicators, and the alcohol content of 10% vol when the total peak area and the total number of peaks of the flavor substances of the characteristic liquor sample were both high and the extraction effect of the flavor substances of the characteristic liquor sample was the best was found as the optimal analytical alcohol content; the extraction effects of flavor substances of liquors with different alcohol content were as shown in the attached manual Figure 2 shown.

[0094] Selection of extraction solvent for characteristic liquor samples: Different solvents have different extraction efficiencies for flavor substances in characteristic liquor samples. Under the optimal analytical alcohol content and other constant conditions, the extraction effects of ethyl acetate, ether, n-hexane, n-butanol, n-pentane, dichloromethane and other solvents on flavor substances in the same characteristic liquor sample were compared; the total peak area and total peak number of liquor flavor substances were used as measurement indicators, and ethyl acetate, which had the largest total peak number and the highest total peak area, was selected as the optimal extraction solvent; the extraction solvent optimization diagram is attached to the instruction manual Figure 3 shown.

[0095] Optimization of the amount of extraction solvent: Under other constant conditions, the effect of the solid-liquid ratio on the extraction effect was investigated. The extraction of flavor substances in the same special wine sample was analyzed when the solid-liquid ratio was 5:1, 5:2, 5:3, 5:4, 5:5, and 5:10. 2 mL of extraction solvent was selected as the optimal amount of extraction agent, that is, the solid-liquid ratio was 5:2; the optimization diagram of the amount of extraction solvent is attached to the instruction manual Figure 4 shown.

[0096] E72: Optimization of instrumental analysis methods

[0097] Instrumental chromatographic column optimization: DB-WAX-UI capillary column, DB-FFAP capillary column, and HP-5 capillary column were compared. The column parameters were all 30m×0.25mm×0.25μm. The total peak area and total peak number of the flavor substances in the wine samples were used as the measurement indicators for the analysis effect. The DB-WAX-UI capillary column with the largest number of extracted flavor substances was selected as the best gas phase capillary column. The instrumental chromatographic column optimization is as shown in the attached manual. Figure 5 shown.

[0098] E73: Flavor substance information and spiked recovery of specialty liquor samples

[0099] The same sensory attribute flavor of the characteristic liquor samples is contributed by the flavor substances with similar sensory characteristics in the formula and the liquor. The flavor substances with similar sensory characteristics are clustered and quantitatively analyzed as follows: a certain concentration gradient of flavor substances is prepared in ethyl acetate solution, 2 μL of citronellol with a concentration of 11727 mg / L is added as the internal standard, the ratio of the peak area of ​​citronellol to the peak area of ​​the internal standard is used as the ordinate, and the concentration ratio is used as the abscissa to draw a standard curve, and the detection limit LOD and the quantification limit LOQ of the flavor substances under the experimental conditions are calculated with the signal-to-noise ratio equal to 3 as the standard; the results are shown in Table 3:

[0100] Table 3 Standard curve parameter information table

[0101]

[0102] F: Combined with the flavor fusion results of the specialty liquor samples, determine the content range of flavor substances representing the sensory attributes in the specialty liquor samples.

[0103] F1: Adaptation to different styles of base wine

[0104] Compare and analyze the compatibility of three different styles of base wines with the medicinal flavors of the formula, and determine the best base wine based on the taste and flavor characteristics of the special wine samples. After sensory evaluation by the expert group, select the base wine used by the special wine sample with the largest comprehensive sensory evaluation score as the best base wine;

[0105] F2: Special wine soaking parameters

[0106] The changes in sensory and physical and chemical indices of the characteristic liquor samples were compared and analyzed under different soaking times of 20 days, 30 days, 40 days and 50 days, and different amounts of functional excipients of 0.5%, 1%, 1.5% and 2% soaking conditions for the same base liquor. The safe and effective content range of the functional factors reported in the literature was compared. Combined with the sensory evaluation results of the expert group, the optimal soaking process was selected, which can not only efficiently and quickly extract the functional factors but also does not affect the sensory flavor fusion of the characteristic liquor samples, with a dosage of 2% and a soaking time of 40 days; the sensory evaluation of the trial samples with different soaking parameters is shown in the attached manual. Figure 6 as shown.

[0107] F3: Analyze the content of representative flavor substances of the characteristic liquor samples with the same sensory attributes in the best soaking process samples, and determine the content range of representative flavor substances of the characteristic liquor samples with the sensory attributes in combination with the flavor fusion results of the characteristic liquor samples;

[0108] F4: Combining the sensory evaluation results of the characteristic wine samples with the content of flavor substances represented by the sensory attributes of the characteristic wine samples, when the sensory evaluation score of the characteristic wine samples reaches 90 points or more, and the range of the characteristic flavor content represented by the sensory attributes is within the range of the sensory attribute content represented by the sensory attributes of the characteristic wine samples determined in F3, it can be determined that the sensory style characteristics of the characteristic wine samples are typical, and the compatibility and integration with the formula are good. The range of the sensory attribute flavor substances of the wine is determined, as shown in Table 4:

[0109] Table 4 Information on the content of characteristic flavor substances in liquor

[0110] Sensory attributes Content range mg / L Plant fragrance 260.70±52.14 Sour 2155.82±431.16 Baking aroma 118.54±23.71 Fruity 26.95±5.39 Sweet 0.31±0.061 Floral scent 24.02±4.80

[0111] The above-mentioned embodiments only express the basic implementation methods of the present invention, and the description thereof is relatively specific and detailed, but it cannot be understood as limiting the scope of the invention patent. It should be pointed out that for ordinary technicians in this field, several variations and improvements can be made without departing from the concept of the present invention, which all belong to the protection scope of the present invention.

Claims

1. A method for developing a flavor-oriented specialty liquor product, characterized in that: The following steps are involved: A: Determine the medicinal flavor of the special wine formula; B: Using liquor as the base liquor, directly soaking a certain amount of the formula, trial-producing special liquor samples, and analyzing the sensory flavors of different special liquor samples through sensory evaluation; C: Comprehensively adopt olfactory and gas chromatography-mass spectrometry analysis technology to analyze the flavor substances of the special wine samples and clarify the flavor substances of the special wine samples and their aroma contribution; D: Comprehensively use olfaction and gas chromatography-mass spectrometry analysis technology to analyze the flavor substances in the special wine formula and clarify the flavor substances in the formula and their aroma contribution; E: Establish a quantitative analysis method for flavor substances in special wine samples to determine the content of flavor substances in special wine samples; F: Combined with the flavor fusion results of the specialty liquor samples, determine the content range of flavor substances representing the sensory attributes in the specialty liquor samples.

2. The method for developing a flavor-oriented specialty liquor product according to claim 1, characterized in that: The method for analyzing the sensory flavors of different wine trial samples by sensory evaluation in step B comprises: B1: Invite 5 national-level wine judges to form an expert panel; B2: Five expert tasters conducted sensory evaluation on the appearance and color (20 points), aroma (30 points), taste and texture (40 points), and style (10 points) of the wine. The average score of the expert tasters was used as the comprehensive sensory evaluation score of the featured wine samples. B3: According to the scoring results, if the comprehensive sensory evaluation score of the characteristic liquor samples is greater than 90 points, it is determined as a good level of liquor flavor adaptability; if the comprehensive sensory evaluation score of the characteristic liquor samples is 80-90 points, it is determined as a general level of liquor flavor adaptability; if the comprehensive sensory evaluation score of the characteristic liquor samples is less than 80 points, it is determined as a poor level of liquor flavor adaptability.

3. The method for developing a flavor-oriented specialty liquor product according to claim 1, characterized in that: The method of step C comprehensively using olfaction and gas chromatography-mass spectrometry analysis technology to analyze the flavor substances of the characteristic liquor sample and clarifying the characteristic flavor substances of the characteristic liquor sample and their aroma contribution includes: C1: Select 7890A-5975C gas chromatograph-mass spectrometer and DB-FFAP capillary column (30m×0.25mm, 0.25μm); select characteristic liquor samples with a comprehensive sensory evaluation score of >90 points; C2: Measure 1 mL of the specialty wine sample into a 10 mL screw-thread bottle, add 9.6 mL of saturated sodium chloride solution, and store at 4 °C for testing; C3: Set up 7890A-5975C gas chromatograph-mass spectrometer and DB-FFAP capillary column (30m×0.25mm, 0.25μm): injection port temperature is 250℃, carrier gas is helium, flow rate is 1mL / min, non-split injection, program temperature rise; 40℃ for 1min, 3℃ / min to 130℃ and hold for 0min, 10℃ / min to 220℃ and hold for 10min; mass spectrometry conditions: EI ion source, electron energy is 70eV, ion source temperature is 230℃, quadrupole temperature is 150℃, solvent delay is 0min, acquisition mode is SIM / Scan, scanning range is m / z 35~550amu; C4: Three professional researchers in the field of liquor flavor and quality were selected to form a sniffing panel. The sniffing panel members smelled the liquor at the sniffing port and recorded the retention time, aroma description and aroma intensity of the characteristic compounds of the sensory attributes. Each person sniffed the same sample three times and the aroma intensity was assessed using a three-point method of 0 to 3 points: "0" for no aroma, "1" for weak aroma intensity, "2" for medium aroma intensity, and "3" for strong aroma intensity. The compounds smelled by all three sniffing panel members with similar sensory descriptions and the average aroma intensity were taken as the analysis results.

4. The method for developing a flavor-oriented specialty liquor product according to claim 1, characterized in that: The method of step D comprehensively using olfaction and gas chromatography-mass spectrometry analysis technology to analyze the flavor substances in the formula of the characteristic liquor and clarifying the flavor substances in the formula and their aroma contribution includes: D1: After grinding the ingredients of the formula, weigh 2g of the ingredients of the formula into a 20mL headspace screw bottle and store at 4℃ for testing; D2: Set up 7890A-5975C gas chromatograph-mass spectrometer and DB-FFAP capillary column (30m×0.25mm, 0.25μm): injection port temperature is 250℃, carrier gas is helium, flow rate is 1mL / min, non-split injection, program temperature rise; 40℃ for 1min, 3℃ / min to 130℃ and hold for 0min, 10℃ / min to 220℃ and hold for 10min; mass spectrometry conditions: EI ion source, electron energy is 70eV, ion source temperature is 230℃, quadrupole temperature is 150℃, solvent delay is 0min, acquisition mode is SIM / Scan, scanning range is m / z 35~550amu; D3: Three professional researchers in the field of liquor flavor and quality were selected to form a sniffing panel. The sniffing panel members smelled the liquor at the sniffing port and recorded the retention time, aroma description and aroma intensity of the characteristic compounds of the sensory attributes. Each person sniffed the same sample three times and the aroma intensity was assessed using the three-point method of 0 to 3 points: "0" means no aroma, "1" means weak aroma intensity, "2" means medium aroma intensity, and "3" means strong aroma intensity. For compounds smelled by all three sniffing panel members and with similar sensory descriptions, the average value of the aroma intensity was taken as the analysis result.

5. The method for developing a flavor-oriented specialty liquor product according to claim 1, characterized in that: The step E establishes a quantitative analysis method for flavor substances in a characteristic liquor sample, and the method for determining the content of flavor substances in a characteristic liquor sample comprises: E1: Select samples, standards, and reagents Sample: Specialty wine samples Standards: acetic acid, propionic acid, butyric acid, 3-methylbutyric acid, isobutyric acid, ethyl phenylacetate, phenylethyl acetate, ethyl 3-phenylpropionate, acetophenone, phenylethanol, ethyl butyrate, ethyl 2-methylbutyrate, ethyl valerate, ethyl octanoate, ethyl lactate, ethyl benzoate, γ-nonalactone, trimethylpyrazine, furfural, 2-acetylfuran, (±)-limonene, α-cedrene, α-cedrol, hexanal, benzaldehyde, citronellol; Reagents: n-butanol (analytical grade), ether (analytical grade), ethanol (analytical grade), n-pentane (chromatographic grade), dichloromethane (chromatographic grade), n-hexane (chromatographic grade), ethyl acetate (chromatographic grade); E2: Select instruments and equipment A 7890A-5975C gas chromatograph-mass spectrometer, an HP-5 capillary column (30 m × 0.25 mm, 0.25 μm), a DB-WAX UI capillary column (30 m × 0.25 mm, 0.25 μm), a DB-FFAP capillary column (30 m × 0.25 mm, 0.25 μm), a DB-5MS capillary column (30 m × 0.25 mm, 0.25 μm), a Mikro220R centrifuge, a VORTEX-GENIE adjustable speed timing vortex mixer, an MS1602TS electronic balance, and a Branson3210 ultrasonic cleaner were used. E3: Measure 5 mL of the specialty liquor sample into a 50 mL centrifuge tube with a scale, add 20 mL of saturated sodium chloride aqueous solution, 2 μL of 11727 mg / L citronellol internal standard, use 2 mL of ethyl acetate, vortex for 1 min, centrifuge and extract, take the upper organic phase, and store it at 4 °C for testing; E4: Chromatographic conditions: Column: HP-5 capillary column (30m×0.25mm, 0.25μm), DB-FFAP capillary column (30m×0.25mm, 0.25μm), DB-WAX UI capillary column (30m×0.25mm, 0.25μm); Temperature program: 40℃ for 1min, 5℃ / min to 230℃ for 10min; Injection port temperature 250℃, carrier gas helium, flow rate 1.0mL / min, splitless injection, injection volume 1μL; E5: Mass spectrometry conditions: electron impact ionization source, electron energy of 70 eV, ion source temperature of 230 °C, quadrupole temperature of 150 °C; solvent delay: 5.0 min, acquisition mode of full scan, scanning range of m / z 35-350 amu; E6: Qualitative and quantitative analysis The retention index of the compound was qualitatively determined by comparing it with the NIST14 spectral library and standard verification; A certain concentration of flavor substance standard solution was prepared with 53% ethanol solution, 5 mL of the standard solution was measured and placed in a 50 mL centrifuge tube with a scale, 20 mL of saturated sodium chloride aqueous solution and 2 μL of citronellol internal standard with a concentration of 11727 mg / L were added, 2 mL of ethyl acetate was used, vortexed for 1 min, centrifuged and extracted, the upper organic phase was taken, and stored at 4°C for testing; a standard curve was established by the mass concentration of the standard sample / internal standard concentration-peak area of ​​the standard solution / peak area of ​​the internal standard; the mass concentration with a chromatographic peak signal-to-noise ratio greater than 3 was determined as the detection limit, and the mass concentration with a signal-to-noise ratio greater than 10 was determined as the quantification limit; E7: Results and Optimization E71: Sample preparation optimization Alcohol content dilution of characteristic liquor: 5 mL of liquor sample was measured and put into a white sample bottle, and different volumes of saturated sodium chloride aqueous solution were added respectively, and the alcohol content of the characteristic liquor sample was diluted to 12% vol, 10% vol, 9% vol, 8% vol, 7% vol, and 6% vol, and 2 μL of citronellol internal standard with a concentration of 11727 mg / L and 2 mL of ethyl acetate were added respectively, and the mixture was vortexed for 1 min, and the upper organic phase was centrifuged to be tested, and the extraction effect of the same extraction solvent on the characteristic liquor flavor substances at different alcohol content was compared; the total peak area and the total peak number of the flavor substances of the characteristic liquor sample were used as the measurement indicators, and the alcohol content of 10% vol when the total peak area and the total peak number of the flavor substances of the characteristic liquor sample were both high and the extraction effect of the flavor substances of the characteristic liquor sample was the best was found as the optimal analytical alcohol content; Selection of extraction solvents for specialty liquor samples: Different solvents have different extraction efficiencies for flavor substances in specialty liquor samples. Under the optimal analytical alcohol content and other constant conditions, the extraction effects of ethyl acetate, ether, n-hexane, n-butanol, n-pentane, dichloromethane and other solvents on flavor substances in the same specialty liquor sample were compared. Taking the total peak area and total peak number of liquor flavor substances as measurement indicators, ethyl acetate, which has the largest total number of extracted peaks and the highest total peak area, was selected as the optimal extraction solvent. Optimization of the amount of extraction solvent: Under other constant conditions, the effect of the solid-liquid ratio on the extraction effect was investigated. The extraction of flavor substances in the same special wine sample was analyzed when the solid-liquid ratio was 5:1, 5:2, 5:3, 5:4, 5:5, and 5:

10. 2 mL of extraction solvent was selected as the optimal amount of extractant, that is, the solid-liquid ratio was 5:2; E72: Optimization of instrumental analysis methods Instrumental chromatographic column optimization: DB-WAX-UI capillary column, DB-FFAP capillary column, and HP-5 capillary column were compared. The column parameters were all 30m×0.25mm×0.25μm. The total peak area and total peak number of the flavor substances in the same special wine sample were used as the measurement indicators for the analysis effect. The DB-WAX-UI capillary column with the largest number of extracted flavor substances was selected as the best gas phase capillary column. E73: Flavor substance information and spiked recovery of specialty liquor samples The same sensory attribute flavor of the special liquor samples is contributed by the flavor substances with similar sensory characteristics in the formula and the liquor. The flavor substances with similar sensory characteristics are clustered and quantitatively analyzed. The steps are: prepare a certain gradient of the flavor substances of the special liquor samples in ethyl acetate solution, add 2μL of citronellol with a concentration of 11727mg / L as the internal standard, draw a standard curve with the ratio of the peak area of ​​citronellol to the peak area of ​​the internal standard as the ordinate, and the concentration ratio as the abscissa, and calculate the detection limit LOD and quantification limit LOQ of the flavor substances under the experimental conditions with the signal-to-noise ratio equal to 3 as the standard.

6. The method for developing a flavor-oriented specialty liquor product according to claim 1, characterized in that: The method for determining the content range of flavor substances represented by the sensory attributes of the characteristic liquor sample in step F in combination with the flavor fusion degree result of the characteristic liquor sample comprises: F1: Adaptation to different styles of base wine Compare and analyze the compatibility of three different styles of base wines with the medicinal flavors of the formula, and determine the best base wine based on the taste and flavor characteristics of the special wine samples. After sensory evaluation by the expert group, select the base wine used by the special wine sample with the largest comprehensive sensory evaluation score as the best base wine; F2: Special wine soaking parameters The changes in sensory and physical and chemical indices of the characteristic liquor samples were compared and analyzed under different soaking times of 20 days, 30 days, 40 days and 50 days, and different soaking amounts of functional excipients of 0.5%, 1%, 1.5% and 2%. The safe and effective content range of the functional factors reported in the literature was compared. Combined with the sensory evaluation results of the expert group, the optimal soaking process was selected, which was 2% and 40 days, which could extract the functional factors efficiently and quickly without affecting the sensory flavor fusion of the characteristic liquor samples. F3: Analyze the content of representative flavor substances of the characteristic liquor samples with the same sensory attributes in the best soaking process samples, and determine the content range of representative flavor substances of the characteristic liquor samples with the sensory attributes in combination with the flavor fusion results of the characteristic liquor samples; F4: Combine the sensory evaluation results of the characteristic liquor samples with the content of flavor substances represented by the sensory attributes of the characteristic liquor samples. When the sensory tasting score of the characteristic liquor samples reaches 90 points or above, and the content range of the characteristic flavor represented by the sensory attributes is within the content range of the flavor substances represented by the sensory attributes of the characteristic liquor samples determined in F3, it can be determined that the sensory style characteristics of the characteristic liquor samples are typical, and have good compatibility and integration with the formula.

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