CN112964816B - Method for detecting volatile flavor substances in rice-flavor liquor - Google Patents
Method for detecting volatile flavor substances in rice-flavor liquor Download PDFInfo
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Abstract
The invention relates to the technical field of liquor detection, and particularly discloses a method for detecting volatile flavor substances in rice-flavor liquor. The detection method of the volatile flavor substances in the rice-flavor liquor comprises the following steps: (1) adsorbing and extracting volatile flavor substances in the rice-flavor liquor by using an extraction needle; (2) inserting the extraction needle into a gas chromatograph to perform gas chromatographic separation; (3) and detecting the components separated by the gas chromatograph by using a detector. The method can successfully detect and measure the content of volatile flavor substances in the rice-flavor liquor; in addition, the method can also screen out the aroma components and the bitter components in the rice-flavor liquor.
Description
Technical Field
The invention relates to the technical field of liquor detection, in particular to a method for detecting volatile flavor substances in rice-flavor liquor.
Background
Chinese liquor is one of the oldest distilled liquors in the world, is recorded as early as the time of Western Han dynasty in China, and is prepared by taking grains (rice, sorghum, wheat and the like) as raw materials and distiller's yeast as a saccharification leavening agent in a solid, semi-solid or liquid fermentation mode through processes of distillation, ageing, blending and the like. Due to the diversity of raw materials, brewing microorganisms, a brewing process and the like, the liquor forms different characteristic odor types, and at present, the liquor in China has 12 odor types, namely, a combination odor type, a phoenix odor type, a sesame odor type, a special odor type, a strong fragrance odor type, a medicinal odor type, a white spirit and a fermented soybean odor type besides four basic odor types, namely, a strong odor type, a Maotai odor type, a fen odor type and a rice odor type. Wherein, the rice-flavor liquor has been publicized as the original liquor of Chinese liquor, and has a brewing history which is more long-term than strong flavor type, Maotai flavor type, fen flavor type and other flavor types. The rice-flavor liquor is represented by Guilin Sanhua liquor, has the characteristics of short production period, elegant rice flavor, soft and soft taste, cool taste and pleasant aftertaste, and is mainly produced in two broad areas, Hunan, Hubei, Fujian and the like.
At present, the research on rice-flavor liquor mainly focuses on the production process, and the research on flavor substances of the rice-flavor liquor is relatively less. Moreover, the research reports about the main aroma components and bitter substances of the rice-flavor liquor are rare.
Disclosure of Invention
Aiming at the defects of the research on the volatile flavor substances in the rice-flavor liquor in the prior art, the invention firstly provides a method for detecting the volatile flavor substances in the rice-flavor liquor.
The technical problem to be solved by the invention is realized by the following technical scheme:
the invention provides a method for detecting volatile flavor substances in rice-flavor liquor, which comprises the following steps:
(1) adsorbing and extracting volatile flavor substances in the rice-flavor liquor by using an extraction needle;
(2) inserting the extraction needle into a gas chromatograph to perform gas chromatographic separation;
(3) detecting the components separated by the gas chromatograph by using a detector;
the specific method for adsorbing and extracting the volatile flavor substances in the rice-flavor liquor by using the extraction needle in the step (1) comprises the following steps:
sucking 5-10 mL of rice-flavor liquor, putting the rice-flavor liquor into a sample bottle, and adding water to dilute the liquor until the alcohol concentration is 10-15% vol; then adding 1-2 g of NaCl, and covering a cover; then placing the sample bottle on a magnetic stirring heater, and preheating for 3-8 min at 40-50 ℃; and inserting an extraction needle, and performing adsorption extraction for 40-60 min.
The inventor finds out in research that one of the difficulties in the process of detecting the volatile flavor substances in the rice-flavor liquor is how to enrich the volatile flavor substances in the rice-flavor liquor as much as possible, so that the method is favorable for comprehensively reflecting the volatile flavor substances in the rice-flavor liquor; the enrichment obtained by different methods has different components. The inventor finds out through a large number of experiments that a large amount of volatile flavor substances can be enriched under the conditions. At least the following volatile flavors are enriched by the above method: methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, β -phenylethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, phenylethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid, and nonanoic acid.
Preferably, the specific method for adsorbing and extracting the volatile flavor substances in the rice-flavor liquor by using the extraction needle in the step (1) comprises the following steps:
adding water to dilute the rice-flavor liquor to an alcohol concentration of 11-13% vol, and sucking 5-7 mL of diluent to place into a sample bottle; then adding 1.2-1.6 g of NaCl, and covering a cover; then placing the sample bottle on a magnetic stirring heater, and preheating for 5-8 min at 40-50 ℃; and inserting an extraction needle, and performing adsorption extraction for 45-55 min.
Preferably, the specific conditions for the gas chromatographic separation in step (2) are: a DB-WAX UI chromatographic column is adopted, the temperature of a sample inlet is 200-280 ℃, no shunt is generated, and helium is used as carrier gas; and separating by adopting a gradient temperature-rising program.
Preferably, the gradient temperature-raising program is: the initial temperature is 30 ℃, the temperature is kept for 6min, the temperature is raised to 40 ℃ at the speed of 2 ℃/min, the temperature is kept for 2min, the temperature is raised to 100 ℃ at the speed of 5 ℃/min, the temperature is kept for 10min, the temperature is raised to 200 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min.
How to separate the volatile flavor substances after the obtained volatile flavor substances are enriched is the second difficulty in the process of detecting the volatile flavor substances in the rice-flavor liquor. If the enriched volatile flavor substances cannot be separated, the components cannot be detected. The inventor of the invention has conducted a great deal of experimental research, and the results show that under the gas chromatography conditions, especially under the gradient temperature rise program, the volatile flavor substances obtained by enrichment can be effectively separated, so that the invention successfully realizes the detection of each component.
Test results show that under the conditions of the gradient temperature-rising program, the gas chromatography conditions can be adopted to ensure that methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid and nonanoic acid can be sufficiently separated, and each component has different retention time. The detection method can successfully detect methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid and nonanoic acid in the rice-flavor liquor.
Preferably, the detector in step (3) is an MS detector; wherein the MS conditions are as follows: selecting an EI ionization source; the ion source temperature is 230 ℃; the electron energy is 70 eV; the acquisition mode is a full scanning mode; the mass scanning range is 50-550 m/z. Under the above gas chromatography conditions, the MS detection conditions allow accurate recognition of methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isopentanol, n-octanol, β -phenethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid, and nonanoic acid in the rice-flavor liquor.
In a second aspect of the present invention, there is provided a method for measuring the content of volatile flavor substances in rice-flavor liquor, wherein the volatile flavor substances to be measured comprise methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, β -phenylethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid, and nonanoic acid;
The method specifically comprises the following steps:
preparing a standard solution: accurately sucking 2.0mL of methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenylethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid and nonanoic acid respectively, placing the mixture into a 100mL volumetric flask, fixing the volume by using ethanol with the volume fraction of 50-70%, and uniformly mixing to obtain a standard stock solution of each component; accurately sucking 0mL, 0.25mL, 0.5mL, 1.0mL, 2.0mL and 4.0mL of standard stock solution of each component, respectively placing the standard stock solution, the 2.0mL and the 4.0mL of standard stock solution in 100mL sample bottles, and performing constant volume by using 50-70% ethanol to obtain standard solutions with different concentration gradients of each component;
and (3) standard curve establishing: accurately sucking 10.0mL of standard solutions with different concentration gradients of each component, and adding 0.10mL of internal standard solutions respectively; loading the sample respectively, and detecting each component by gas chromatography; establishing a standard curve of each component by taking the concentration ratio of each component to the internal standard substance as a horizontal coordinate and the peak area ratio of each component to the internal standard substance as a vertical coordinate;
The content determination method of the volatile flavor substances in the rice-flavor liquor comprises the following steps: accurately sucking 10.0mL of rice-flavor liquor, adding 0.10mL of internal standard solution, uniformly mixing, loading, and detecting the peak area ratio of each volatile flavor substance to the internal standard substance by using gas chromatography; and substituting the peak area ratio of each volatile flavor substance to the internal standard substance into each component standard curve to obtain the concentration of each volatile flavor substance.
The content determination method provided by the invention realizes simultaneous determination of the content of methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid and nonanoic acid in the rice-flavor liquor for the first time.
Preferably, the internal standard solution is prepared by the following method: accurately sucking 2.0mL of n-amyl acetate, diluting to 100mL by using 60% (v/v) ethanol solution, uniformly mixing, and preparing an internal standard solution with the volume fraction of 2%.
Preferably, the gas chromatography conditions in the standard curve establishing step are the same as those in the content measuring step of the volatile flavor substances in the rice-flavor liquor.
The gas chromatography conditions are as follows: a DB-WAX UI chromatographic column is adopted; the sample inlet temperature is 200-250 ℃, the sample injection amount is 0.8-1.5 mu L, the split ratio is 100: 1-3, the flow rate is 0.8-1.5 mL/min, and the temperature of an FID detector is 200-250 ℃; hydrogen (H2): air (O2): tail blow (N2) 40:400: 25; and separating by adopting a gradient temperature-rising program.
Preferably, the gas chromatography conditions are: a DB-WAX UI chromatographic column is adopted; the sample inlet temperature is 220 ℃, the sample injection amount is 1 mu L, the split ratio is 100:1, the flow rate is 1mL/min, and the temperature of an FID detector is 220 ℃; hydrogen (H2): air (O2): the tail blow (N2) was 40:400: 25.
Preferably, the gradient temperature-raising program is: the initial temperature is 30 ℃, the temperature is kept for 6min, the temperature is raised to 40 ℃ at the speed of 2 ℃/min, the temperature is kept for 2min, the temperature is raised to 100 ℃ at the speed of 5 ℃/min, the temperature is kept for 10min, the temperature is raised to 200 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min.
In the research process of the inventor, the difficulty in measuring the content of methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenylethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid and nonanoic acid in the rice-flavor liquor is how to separate the components. The content determination of each component can be realized only by successfully separating each component by adopting a gas chromatograph so that each component has different retention time. Whether each component can be successfully separated is closely related to the gas chromatography condition, particularly to the gradient temperature rise program in the gas chromatography.
The inventors have conducted extensive experiments and research, and as a result, the inventors have shown that under the above-mentioned gas chromatography conditions, especially under the above-mentioned gradient temperature-raising program, methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, β -phenylethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, phenylethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid, and nonanoic acid in rice-flavor liquor can be effectively and sufficiently separated, so that each component has different retention times; thereby successfully realizing the content measurement of each component.
The third aspect of the invention provides application of a content determination method of volatile flavor substances in rice-flavor liquor in screening aroma components and bitter components in the rice-flavor liquor.
Based on the content determination method of the volatile flavor substances in the rice-flavor liquor, the invention successfully screens out the aroma components and the bitter components in the rice-flavor liquor for the first time by combining OAV and DoT.
Has the advantages that: the invention provides a brand new method for detecting volatile flavor substances in rice-flavor liquor, which realizes the detection and content determination of volatile flavor substances such as methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, phenethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, caprylic acid, capric acid, pelargonic acid and the like for the first time; in addition, the invention successfully screens out the aroma components and the bitter components in the rice-flavor liquor for the first time.
Detailed Description
The present invention will be described in further detail with reference to specific examples, but the present invention is not limited to these examples in any way.
Experimental raw materials, main reagents and main equipment designed in the following examples are shown in tables 1-3; other non-disclosed materials, reagents and equipment are all conventional in the art in the examples.
TABLE 1 Experimental materials
TABLE 2 major reagents
TABLE 3 Main Equipment
Example 1 detection method of volatile flavor substances in rice-flavor liquor
(1) Extracting volatile flavor substances in rice-flavor liquor by using extraction needle
The specific method of the step is as follows: adding water to dilute the rice-flavor liquor until the alcohol concentration is 12% vol, and sucking 5mL of diluent to place into a sample bottle; then 1.4g NaCl was added and the lid was closed; then placing the sample bottle on a magnetic stirring heater, and preheating for 5min at 45 ℃; then inserting an extraction needle, and performing adsorption extraction for 50 min; extraction needle before insertion the extraction needle (50/30 μm DVB/CAR/PDMS) was activated at 250 ℃ for 10 min.
(2) Inserting the extraction needle into gas chromatograph for gas chromatographic separation
The specific method of the step is as follows: DB-WAX UI chromatographic column (30m × 0.25mm × 0.25 μm, Agilent corporation, USA) is adopted, the injection port temperature is 250 ℃, no shunt is carried out, and helium is used as carrier gas; separating by adopting a gradient temperature program; the gradient temperature-raising program comprises the following steps: the initial temperature is 30 ℃, the temperature is kept for 6min, the temperature is raised to 40 ℃ at the speed of 2 ℃/min, the temperature is kept for 2min, the temperature is raised to 100 ℃ at the speed of 5 ℃/min, the temperature is kept for 10min, the temperature is raised to 200 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min.
(3) Detecting the components separated by the gas chromatograph by using a detector
The specific method of the step is as follows: the detector is an MS detector; wherein the MS conditions are as follows: selecting an EI ionization source; the ion source temperature is 230 ℃; the electron energy is 70 eV; the acquisition mode is a full scanning mode; the mass scanning range is 50-550 m/z.
By adopting the method, volatile flavor substances such as methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid and nonanoic acid in the rice-flavor liquor can be enriched and enriched; as can be seen from the retention times in table 4, the volatile flavors can be well separated under the gas chromatography conditions of the present invention, and each component has a different retention time, so that the method can accurately detect the components.
The test materials in Table 1 were further tested by the method of example 1, and the test results are shown in Table 5.
Table 4 retention time of volatile flavour substances
TABLE 5 detection of volatile flavor components in Rice-flavored Baijiu from different sources
Note: "+" indicates that the substance was detected, and "-" indicates no detection.
As can be seen from table 5, 30 flavors were identified in 9 rice-flavor white spirits by the method described in example 1, including 17 esters, 5 alcohols, 4 aldehydes, 1 ketone and 3 others, wherein 9 flavors including ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl decanoate, furfural, benzaldehyde, ethyl nonanoate, diethyl succinate and ethyl palmitate were common volatile flavors of the 9 rice-flavor white spirits. The method for detecting volatile flavor substances in rice-flavor liquor described in example 1 can be used for identifying the source of each rice-flavor rice wine and controlling the production quality of the rice-flavor liquor in each rice-flavor liquor factory.
Example 2 measurement of content of volatile flavor substances in Rice-flavor liquor
(1) Preparing a standard solution: accurately sucking 2.0mL of each of methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenylethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid and nonanoic acid, placing the mixture into a 100mL volumetric flask, fixing the volume by using ethanol with the volume fraction of 60%, and uniformly mixing to obtain a standard stock solution of each component; accurately sucking 0mL, 0.25mL, 0.5mL, 1.0mL, 2.0mL and 4.0mL of standard stock solution of each component, respectively placing in a 100mL sample bottle, and fixing the volume with 60% ethanol to obtain standard solutions of different concentration gradients of each component;
(2) And (3) standard curve establishing: accurately sucking 10.0mL of standard solutions with different concentration gradients of each component, and adding 0.10mL of internal standard solutions respectively; loading the sample respectively, and detecting each component by gas chromatography; establishing a standard curve of each component by taking the concentration ratio of each component to the internal standard substance as a horizontal coordinate and the peak area ratio of each component to the internal standard substance as a vertical coordinate;
(3) the content determination method of the volatile flavor substances in the rice-flavor liquor comprises the following steps: accurately sucking 10.0mL of rice-flavor liquor, adding 0.10mL of internal standard solution, uniformly mixing, loading, and detecting the peak area ratio of each volatile flavor substance to the internal standard substance by using gas chromatography; and substituting the peak area ratio of each volatile flavor substance to the internal standard substance into each component standard curve to obtain the concentration of each volatile flavor substance.
The internal standard solution described in the steps (1) and (2) is prepared by the following method: accurately sucking 2.0mL of n-amyl acetate, diluting to 100mL by using 60% (v/v) ethanol solution, uniformly mixing, and preparing an internal standard solution with the volume fraction of 2%.
And (3) establishing a standard curve in the step (2) and determining the gas chromatography condition in the step (3) to be the same as the gas chromatography condition in the step of determining the content of the volatile flavor substances in the rice-flavor liquor.
The gas chromatography conditions are as follows: DB-WAX UI column (30 m.times.0.25 mm.times.0.25 μm, Agilent Corp., USA); the sample inlet temperature is 220 ℃, the sample injection amount is 1 mu L, the split ratio is 100:1, the flow rate is 1mL/min, and the temperature of an FID detector is 220 ℃; hydrogen (H) 2 ): air (O) 2 ): tail blowing (N) 2 ) 40:400: 25; the gradient temperature program of the gas chromatography is as follows: the initial temperature is 30 deg.C, and the temperature is kept for 6min at 2 deg.CHeating to 40 deg.C/min for 2min, heating to 100 deg.C/min at 5 deg.C/min for 10min, heating to 200 deg.C/min at 10 deg.C/min, and maintaining for 10 min.
The standard curve and retention time for each of the volatile flavors obtained using the method described in example 2 are shown in table 6. The test materials in Table 1 were tested as described in example 2, and the results are shown in Table 7.
TABLE 6 Standard Curve and Retention time for each volatile flavor
As can be seen from table 6, under the above gas chromatography conditions, especially under the above gradient temperature-rising procedure, methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, β -phenylethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, phenylethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid, and nonanoic acid in the rice-flavor liquor can be effectively and sufficiently separated, so that each component has different retention time; and all the components have good linear relation; the content measurement method described in example 2 can be used to measure the content of each component.
TABLE 7 Mass concentrations of volatile flavor components in Rice-flavored Chinese liquor from different sources
Note: "-" indicates that the mass concentration of the flavor substance was not detected.
According to the measurement results of table 7 for the content of the flavor substances of the rice-flavor liquor, 14 flavor substances with the detection rate of more than 50% in 9 rice-flavor liquors are selected, and the content is arranged from high to low: ethyl lactate, isoamyl alcohol, acetic acid, isobutyl alcohol, ethyl acetate, n-propanol, acetal, beta-phenylethyl alcohol, acetaldehyde, pelargonic acid, ethyl pelargonate, n-butanol, decanoic acid and octanoic acid, which are main flavor substances in the rice-flavor white spirit. Wherein two esters of ethyl acetate and ethyl lactate exist in 9 rice-flavor liquor, the contents of the two esters generally have little difference in the rice-flavor liquor in Guangdong region, and the content of ethyl lactate in the rice-flavor liquor in Guangxi region is far higher than the content of ethyl acetate; in the detection results of the flavor substances, the n-propanol, the isobutanol and the isoamylol are alcohol substances with the highest content in 9 types of rice-flavor liquor, and the isoamylol content is the highest among the three; acetaldehyde and acetal are main aldehyde substances in the rice-flavor liquor; acetic acid and lactic acid are the two acids with the highest content.
Based on the mass concentrations of volatile flavor components in the rice-flavor liquor from different sources in table 7 obtained by the content measurement method described in example 2, the OAV value and OAV value of flavor components in the rice-flavor liquor were calculated. The results of the calculations are shown in tables 8 and 9.
TABLE 8 analysis of OAV of volatile flavor substances in Rice-flavor Chinese spirits from different sources
Note: "-" indicates that the substance concentration was not detected and the OAV value could not be calculated; blank indicates that the threshold for the substance was not found. Threshold references (zhangqian et al, 2019; Fan et al, 2015; van et al, 2011; reiden 29153, et al, 2001).
Generally, substances having an OAV value of 1 or more are considered to be important aroma components, and as is clear from table 8, among 9 types of finished rice-flavor liquor, 12 types of flavor substances having an OAV value of 1 or more are acetaldehyde, ethyl acetate, n-propanol, isobutanol, n-butanol, isoamyl alcohol, ethyl lactate, acetic acid, ethyl nonanoate, β -phenylethyl alcohol, octanoic acid, and nonanoic acid, which are important aroma components in rice-flavor liquor.
TABLE 9 DoT analysis of volatile flavor substances in rice-flavor Chinese spirits from different sources
Note: "-" indicates that the substance concentration was not detected and the OAV value could not be calculated. Bitter taste threshold reference (royal yinye, 2018).
When the DoT of a substance is < 1, it indicates that the substance may not contribute to the sensation of mouth; when DoT is not less than 1, it is indicated that it contributes to taste, and as can be seen from Table 9, in 9 kinds of rice-flavor liquor finished products, the bitter taste DoT of isoamyl alcohol and isobutyl alcohol is not less than 1, indicating that these two substances are the main components causing bitter taste in rice-flavor liquor.
Claims (2)
1. A method for measuring the content of volatile flavor substances in rice-flavor liquor is characterized in that the volatile flavor substances to be measured comprise methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, phenethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid and nonanoic acid;
the method specifically comprises the following steps:
preparing a standard solution: accurately sucking 2.0 mL of methanol, n-propanol, n-butanol, isobutanol, n-pentanol, isoamyl alcohol, n-octanol, beta-phenylethyl alcohol, ethyl acetate, isoamyl acetate, ethyl hexanoate, ethyl heptanoate, ethyl octanoate, ethyl nonanoate, ethyl benzoate, diethyl succinate, ethyl acetate, ethyl palmitate, ethyl oleate, ethyl lactate, acetaldehyde, acetal, furfural, benzaldehyde, acetophenone, acetic acid, octanoic acid, decanoic acid and nonanoic acid respectively, placing the mixture into a 100 mL volumetric flask, fixing the volume by using ethanol with the volume fraction of 50-70%, and uniformly mixing to obtain a standard stock solution of each component; accurately sucking 0 mL, 0.25 mL, 0.5 mL, 1.0 mL, 2.0 mL and 4.0 mL of standard stock solution of each component, respectively placing the standard stock solution, the 2.0 mL and the 4.0 mL of standard stock solution in 100 mL sample bottles, and performing constant volume by using 50-70% ethanol to obtain standard solutions with different concentration gradients of each component;
And (3) standard curve establishing: accurately sucking 10.0 mL of standard solutions with different concentration gradients of each component, and adding 0.10 mL of internal standard solutions respectively; loading the sample respectively, and detecting each component by gas chromatography; establishing a standard curve of each component by taking the concentration ratio of each component to the internal standard substance as a horizontal coordinate and the peak area ratio of each component to the internal standard substance as a vertical coordinate;
the content determination method of the volatile flavor substances in the rice-flavor liquor comprises the following steps: accurately sucking 10.0 mL of rice-flavor liquor, adding 0.10 mL of internal standard solution, uniformly mixing, loading, and detecting the peak area ratio of each volatile flavor substance to the internal standard substance by using gas chromatography; substituting the peak area ratio of each volatile flavor substance to the internal standard substance into each component standard curve to obtain the concentration of each volatile flavor substance;
the gas chromatography condition in the standard curve establishing step is the same as the gas chromatography condition in the rice-flavor liquor volatile flavor substance content measuring step;
the gas chromatography conditions are as follows: a DB-WAX UI chromatographic column is adopted; the sample inlet temperature is 200-250 ℃, the sample injection amount is 0.8-1.5 mu L, the split ratio is 100: 1-3, the flow rate is 0.8-1.5 mL/min, and the temperature of an FID detector is 200-250 ℃; hydrogen gas: air: blowing nitrogen at the tail at a ratio of 40:400: 25; separating by adopting a gradient temperature-raising program;
The gradient temperature-raising program comprises the following steps: the initial temperature is 30 ℃, the temperature is kept for 6 min, the temperature is raised to 40 ℃ at the speed of 2 ℃/min, the temperature is kept for 2 min, the temperature is raised to 100 ℃ at the speed of 5 ℃/min, the temperature is kept for 10 min, the temperature is raised to 200 ℃ at the speed of 10 ℃/min, and the temperature is kept for 10 min.
2. The method for measuring the content of volatile flavor substances in rice-flavor liquor as claimed in claim 1, which is applied to screening of aroma components and bitter components in rice-flavor liquor.
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