CN115656447A - Method for preparing solutions with different fragrances in white spirit - Google Patents
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- 239000003205 fragrance Substances 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000126 substance Substances 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 14
- 235000019568 aromas Nutrition 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 7
- 238000004817 gas chromatography Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 54
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- DLLJVQNYBYOKGS-UHFFFAOYSA-N ethoxyethane;pentane Chemical compound CCCCC.CCOCC DLLJVQNYBYOKGS-UHFFFAOYSA-N 0.000 claims description 10
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 7
- 238000000605 extraction Methods 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 5
- 230000001476 alcoholic effect Effects 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 claims description 4
- 238000007664 blowing Methods 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 239000012141 concentrate Substances 0.000 claims description 2
- 238000010790 dilution Methods 0.000 claims description 2
- 239000012895 dilution Substances 0.000 claims description 2
- 238000011002 quantification Methods 0.000 claims description 2
- 239000000796 flavoring agent Substances 0.000 abstract description 9
- 235000019634 flavors Nutrition 0.000 abstract description 9
- 238000007865 diluting Methods 0.000 abstract description 5
- 239000000523 sample Substances 0.000 description 24
- 238000011156 evaluation Methods 0.000 description 9
- 235000014101 wine Nutrition 0.000 description 7
- 238000001514 detection method Methods 0.000 description 6
- 240000006394 Sorghum bicolor Species 0.000 description 5
- 235000011684 Sorghum saccharatum Nutrition 0.000 description 5
- 239000007789 gas Substances 0.000 description 5
- 230000001953 sensory effect Effects 0.000 description 5
- 239000012071 phase Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000012159 carrier gas Substances 0.000 description 2
- 235000019219 chocolate Nutrition 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
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- 238000002290 gas chromatography-mass spectrometry Methods 0.000 description 2
- 239000001307 helium Substances 0.000 description 2
- 229910052734 helium Inorganic materials 0.000 description 2
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 2
- 239000012528 membrane Substances 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 238000002470 solid-phase micro-extraction Methods 0.000 description 2
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- 238000004821 distillation Methods 0.000 description 1
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- 238000010438 heat treatment Methods 0.000 description 1
- 238000004811 liquid chromatography Methods 0.000 description 1
- 235000001035 marshmallow Nutrition 0.000 description 1
- 238000004451 qualitative analysis Methods 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 239000012088 reference solution Substances 0.000 description 1
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- 230000000638 stimulation Effects 0.000 description 1
- 235000020097 white wine Nutrition 0.000 description 1
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Abstract
The invention discloses a method for preparing solutions with different aromas in white spirit, and belongs to the chemical field of white spirit flavor. The preparation method of the solution with different fragrances in the white spirit comprises the following steps: after the concentrated solution is obtained by the steps of diluting, extracting and concentrating the white spirit, preparing the concentrated solution by adopting a semi-preparative high performance liquid chromatograph, collecting fractions containing different fragrances, then qualitatively and quantitatively preparing different prepared fragrance substances by combining a smell instrument and a gas chromatography mass spectrometer, and finally respectively preparing fragrance solutions according to the quantitation to obtain different fragrance solutions in the white spirit. The method can separate different aroma substances in the white spirit, can intuitively, specifically and accurately express the flavor characteristics of different types of white spirit samples in different years, and can effectively solve the problem that the existing preparation method of aroma solution in the white spirit can not accurately restore the aroma with different flavors in the white spirit.
Description
Technical Field
The invention belongs to the field of liquor flavor chemistry, and particularly relates to a method for preparing solutions with different aromas in liquor.
Background
Chinese liquor is a traditional distilled liquor fermented by grains, different distiller's yeast, fermentation and distillation processes can generate different aroma substances in various types of liquor, and sensory indexes of the Chinese liquor are the main factors for judging the quality and the quality of the liquor. The liquor sensory evaluation detection technology is a stimulation feeling fed back to the brain by human sensory organs, so that the liquor sensory evaluation detection technology cannot be replaced by instrument detection at present, and liquor enterprises need professional evaluation personnel, and the evaluation personnel need to strengthen learning constantly, continuously enlarge knowledge storage and improve accurate and standard evaluation capability.
The judgment of the aroma substances is a key point in the training process of the appraisers, so that the preparation of different aroma solutions in the white spirit is extremely important. For example, the invention CN103351948A discloses a preparation method of a sorghum fragrance reference solution for liquor evaluation, sorghum is used as a raw material to extract sorghum fragrance, and after the extract is clarified, concentrated, adjusted in alcohol concentration and added with a stabilizer, a nose with sorghum fragrance is formed, which is convenient for professionals and common consumers to be more familiar with sorghum fragrance. For example, the invention CN103823033A discloses an analysis and detection method for flavor compounds in white spirit, in the invention, aroma substances in white spirit samples at different time periods are collected by a liquid chromatograph and evaluation of professionals, and then the aroma substances are analyzed and detected by a gas chromatograph to prepare a 'quxiang' solution.
Although the above patent realizes the preparation of the special aroma solution in the white spirit to a certain extent, the following disadvantages still exist: (1) the preparation of the aroma solution in the white spirit is based on the content of aroma substances in the white spirit as much as possible, and the aroma substances extracted from the raw materials cannot accurately restore the aroma concentration in the white spirit, so that the 'aroma substances' in the white spirit cannot be directly known and defined by professionals and common consumers; (2) a white spirit sample is not concentrated, so that when aroma substances in the white spirit are prepared by a liquid chromatograph, the content of some substances is low and the substances cannot be collected; (3) collecting the aroma for different time periods may result in some compounds with low thresholds being taste masked by other tastes during the time period.
Therefore, the field needs a preparation method of aroma solution which can accurately restore different flavors in the white spirit.
Disclosure of Invention
The invention aims to solve the technical problem that the existing preparation method of the aroma solution in the white spirit can not accurately restore the aroma with different flavors in the white spirit.
The technical scheme adopted by the invention for solving the technical problems is as follows: the preparation method of the solutions with different fragrances in the white spirit comprises the steps of diluting, extracting and concentrating the white spirit to obtain concentrated solution, preparing the concentrated solution by adopting a semi-preparative high performance liquid chromatograph, collecting fractions containing different fragrances, then qualitatively and quantitatively preparing different fragrance substances by using a sniffing instrument and combining a gas chromatography mass spectrometer, and finally respectively preparing the fragrance solutions according to the quantitation to obtain the solutions with different fragrances in the white spirit.
The dilution is to take 10-50mL of white spirit sample, and dilute the white spirit sample by saturated salt water until the alcoholic strength is 1-10%.
The extraction is carried out by extracting the diluted white spirit sample by using ether-pentane solution for three times, wherein each extraction time is 5-10min.
Further, the volume ratio of the ether to the pentane in the ether-pentane solution is 1: 1.
Further, the volume ratio of the diethyl ether-pentane solution to the diluted white spirit sample is 3-4: 6-7.
The concentration is to concentrate the extract by a nitrogen blowing instrument to obtain 0.5-1mL of concentrated solution.
The specific method for preparing the solutions with different fragrances in the white spirit comprises the following steps: according to the content of different aroma substances in the white spirit, the different aroma substances are respectively dissolved in the ethanol solution with the same concentration as the ethanol in the original white spirit sample, and the white spirit is bottled and stored.
The beneficial effects of the invention are: according to the technical scheme, concentrated liquor samples are directly used as aroma extracts, different aroma substances in the liquor can be separated as much as possible, qualitative and quantitative effects are achieved, and different aroma solutions are prepared finally.
A single aroma component cannot be well presented in the white spirit, while the aroma in the white spirit prepared by the method in the prior art cannot be well restored, and the various aroma solutions prepared by the method can enable professional sensory evaluation personnel and ordinary consumers to better recognize different aroma characteristics in the white spirit.
Drawings
FIG. 1 is a semi-preparative chromatogram of a wuliangye wine base sample according to an embodiment of the present invention;
FIG. 2 is a gas chromatogram of fraction number F10 chocolate, nut aroma of an example of the invention;
FIG. 3 is a gas chromatogram of fraction number F30 marshmallow aroma of an example of the invention.
Detailed Description
The technical solution of the present invention can be specifically implemented as follows.
The preparation method of the solutions with different aromas in the white spirit specifically comprises the following steps:
(1) Diluting: taking 10-50mL of a white spirit sample, and diluting the white spirit sample by using saturated salt water until the alcoholic strength is 1% -10%;
(2) Extraction: extracting the white spirit sample by using an ether-pentane (1: 1 v/v) solution for three times, wherein each extraction time is 5-10min, and the volume ratio of the ether-pentane solution to the diluted white spirit sample is 3-4: 6-7.
(3) And (3) concentrating: concentrating the extract liquor by a nitrogen blowing instrument to finally obtain 0.5-1mL of sample concentrated solution;
(4) Preparation: preparing the concentrated sample by using a semi-preparative high performance liquid chromatograph, and collecting fractions containing different kinds of aromas;
(5) And (3) characterization: the prepared different aroma substances are characterized by using a sniffer combined with a gas chromatography mass spectrometer;
(6) And (3) quantification: accurately quantifying the prepared different aroma substances by using a gas chromatography mass spectrometer;
(7) Preparation: and (2) according to the content of the aroma substances in the white spirit, dissolving different aroma substances in an ethanol solution (the concentration of the ethanol solution is the same as that of the ethanol in the white spirit sample in the step (1)), and bottling for storage.
The technical solution and effects of the present invention will be further described below by way of practical examples.
Examples
The preparation method of the solutions with different fragrances in the white spirit comprises the following specific experimental steps:
(1) Taking 50mL of wuliangye raw wine with the alcoholic strength of 70%, diluting the wuliangye raw wine with saturated salt water until the alcoholic strength is 10%, wherein the volume of a diluted raw wine sample is 350mL;
(2) Extracting the white spirit sample by using an ether-pentane (1 v/v) solution for three times (70, 60mL), wherein the volume ratio of the ether-pentane solution to the diluted white spirit sample is 4: 7, and each extraction is carried out for 5min, so as to obtain 200mL of extract liquor;
(3) Concentrating the extract liquor by a nitrogen blowing instrument to finally obtain 1mL of sample concentrated solution;
(4) Preparing a concentrated sample by using a semi-preparative high performance liquid chromatograph, and collecting fractions containing different types of aromas, wherein the specific liquid chromatography condition parameters are as follows:
a chromatographic column: watersatlantis T3 OBD Prep (10 mm. Times.250 mm. Times.5 μm); column temperature: 35 ℃; flow rate: 2mL/min; sample introduction amount: 500 mu L of the solution; a detector: DAD detector (220,254nm); elution procedure: the mobile phase A is water, and the mobile phase B is ethanol; 0min, A100. 8min, A80%; 28min, A50%; 40min, A0%;60min, A0%;
the semi-preparative chromatogram of the wuliangye wine base sample in this example is shown in fig. 1, and it can be seen from the graph that: under elution of mobile phases with different proportions, a plurality of chromatographic peaks appear, which indicates that the method can directly separate a plurality of flavor substances in a wuliangye raw wine sample, collect fractions according to the peaks, finally collect 34 special fractions in total, and perform sensory evaluation by professional evaluators, wherein the aroma description is shown in table 1;
TABLE 134 distillate aroma profiles
(5) Taking two special aromas (F10 and F30) as an example, the two aroma components are respectively characterized by combining a sniffer with a gas chromatography mass spectrometer (GC-O-MS), the qualitative results are shown in Table 2, and relevant condition parameters are as follows:
a capillary chromatographic column: HP-INNOWAX,60 m.times.0.32 mm (internal diameter). Times.0.5 μm (membrane thickness) or equivalent chromatography column; sample inlet temperature: 240 ℃; column temperature: initial temperature of 40 deg.C, maintaining for 2min, and raising temperature to 240 deg.C at 5 deg.C/min, and maintaining for 15min; carrier gas: helium with purity not less than 99.999% and flow rate of 1mL/min; an ionization mode: electron impact source (EI) with energy of 70eV; quadrupole rod temperature: 150 ℃; ion source temperature: 230 ℃; transmission line temperature: 250 ℃; timing events: MS closing at 11.5min and MS opening at 15.0 min; and (3) sample introduction mode: a non-shunting mode; the detection mode is as follows: full SCAN mode (SCAN); scanning range: 35.00-350.00amu;
(6) The aroma components of F10 and F30 were further quantified by using gas chromatography mass spectrometry, and the quantitative results are shown in table 2, and the relevant pretreatment and gas chromatography mass spectrometry condition parameters are as follows:
solid Phase Microextraction (SPME): balancing for 15min at 60 ℃; extracting at 60 deg.C for 45min; desorbing at 250 deg.C for 3min.
A capillary chromatographic column: HP-INNOWAX,60 m.times.0.32 mm (inside diameter). Times.0.5 μm (membrane thickness) or equivalent chromatographic column; sample inlet temperature: 250 ℃; column temperature: maintaining the initial temperature at 40 deg.C for 3min, and heating to 230 deg.C at 4 deg.C/min for 10min; carrier gas: helium with purity not less than 99.999% and flow rate of 1mL/min; ionization mode: electron impact source (EI) with energy of 70eV; temperature of the quadrupole rods: 150 ℃; ion source temperature: 230 ℃; transmission line temperature: 250 ℃; and (3) sample introduction mode: a non-shunting mode; the detection mode is as follows: full SCAN mode (SCAN); scanning range: 35.00-350.00amu;
TABLE 2 qualitative and quantitative analysis results of F10 and F30 aroma components
The gas chromatogram of fraction number F10 chocolate and nut aroma is shown in FIG. 2; the gas chromatogram of fraction number F30 cotton candy aroma is shown in FIG. 3;
(7) According to the content of the F10 and F30 aroma substances in the wuliangye raw wine, respectively dissolving the two aroma substances in 70% ethanol solution, bottling and storing to obtain different aroma solutions in the white wine.
According to the embodiment of the invention, the method can accurately prepare the aroma substance solution in the white spirit, so that the flavor characteristics of the white spirit are more intuitively presented.
Claims (7)
1. The preparation method of the solution with different fragrances in the white spirit is characterized in that: after the white spirit is diluted, extracted and concentrated to obtain concentrated solution, a semi-preparative high performance liquid chromatograph is adopted to prepare the concentrated solution and collect fractions containing different aromas, then a smell instrument is combined with a gas chromatography mass spectrometer to qualitatively and quantitatively prepare aroma solutions according to the quantification, and finally the aroma solutions in the white spirit are respectively prepared.
2. The method for preparing the solutions with different fragrances in the white spirit according to claim 1, which is characterized in that: the dilution is to take 10-50mL of white spirit sample, and dilute the white spirit sample by saturated salt water until the alcoholic strength is 1-10%.
3. The method for preparing the solutions with different fragrances in the white spirit according to claim 1, which is characterized in that: the extraction is carried out by extracting the diluted white spirit sample by using an ether-pentane solution for three times, wherein each extraction is carried out for 5-10min.
4. The method for preparing the solutions with different fragrances in the white spirit according to claim 3, wherein the method comprises the following steps: the volume ratio of the diethyl ether to the pentane in the diethyl ether-pentane solution is 1: 1.
5. The method for preparing the solutions with different fragrances in the white spirit according to claim 3, which is characterized in that: the volume ratio of the diethyl ether-pentane solution to the diluted white spirit sample is 3-4: 6-7.
6. The method for preparing the solutions with different fragrances in the white spirit according to claim 1, which is characterized in that: the concentration is to concentrate the extract liquor by a nitrogen blowing instrument to obtain 0.5-1mL of concentrated solution.
7. The method for preparing the solutions with different fragrances in the white spirit according to claim 1, which is characterized in that: the specific method for preparing the solutions with different fragrances in the white spirit comprises the steps of respectively dissolving the substances with different fragrances in the white spirit in an ethanol solution with the same concentration as the ethanol in the original white spirit sample, and bottling for storage.
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103351948A (en) * | 2013-02-01 | 2013-10-16 | 中国食品发酵工业研究院 | Preparation method of Kaoliang liquor fragrance characteristic fragrance reference solution in liquor evaluation |
| CN108303482A (en) * | 2018-02-13 | 2018-07-20 | 江南大学 | A kind of method of extracting and developing and volatility bitter taste substance in identification white wine |
| CN112834639A (en) * | 2020-12-31 | 2021-05-25 | 宜宾五粮液股份有限公司 | Series connection method of solid phase extraction columns for separating volatile ester flavor substances in white spirit |
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- 2022-11-04 CN CN202211375144.6A patent/CN115656447A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103351948A (en) * | 2013-02-01 | 2013-10-16 | 中国食品发酵工业研究院 | Preparation method of Kaoliang liquor fragrance characteristic fragrance reference solution in liquor evaluation |
| CN108303482A (en) * | 2018-02-13 | 2018-07-20 | 江南大学 | A kind of method of extracting and developing and volatility bitter taste substance in identification white wine |
| CN112834639A (en) * | 2020-12-31 | 2021-05-25 | 宜宾五粮液股份有限公司 | Series connection method of solid phase extraction columns for separating volatile ester flavor substances in white spirit |
Non-Patent Citations (1)
| Title |
|---|
| WENLAI FAN等: "Characterization of Aroma Compounds of Chinese "Wuliangye" and "Jiannanchun" Liquors by Aroma Extract Dilution Analysis", J. AGRIC. FOOD CHEM., vol. 54, 3 March 2006 (2006-03-03), pages 5 - 6 * |
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