CN115656447A - Preparation method of different aroma solutions in liquor - Google Patents

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

Preparation method of different aroma solutions in liquor

technical field

The invention belongs to the field of liquor flavor chemistry, and in particular relates to a preparation method of different aroma solutions in liquor.

Background technique

Chinese baijiu is a traditional distilled wine fermented from grains. Different koji, fermentation and distillation processes will produce different aroma substances in various types of baijiu. The sensory indicators are the most important factors to judge the quality and quality of baijiu. Liquor sensory evaluation testing technology is a stimulating feeling that human sensory organs give feedback to the brain, so it cannot be replaced by instrumental testing. Therefore, liquor companies need more professional tasters, and tasters must always strengthen their studies and continuously expand their knowledge reserves. , Improve the ability of accurate and standardized comments.

The determination of aroma substances is a major focus in the training process of tasters, so it is extremely important to make different aroma solutions in liquor. For example, the invention CN103351948A discloses a method for preparing a sorghum aroma reference solution used in liquor evaluation. The sorghum aroma is extracted from sorghum as a raw material. The wine nose of aroma makes it easier for professionals and ordinary consumers to be more familiar with "sorghum fragrance". For example, the invention CN103823033A discloses a method for the analysis and detection of flavor compounds in liquor. The invention collects the aroma substances of liquor samples in different time periods through liquid chromatography and professional evaluation, and then analyzes and detects the aroma substances through a GC-MS instrument. Make the "koji" solution.

Although the above-mentioned patent has realized the making of special aroma solution in liquor to a certain extent, there are still the following disadvantages: 1. the making of aroma solution in liquor should be based on the aroma substance content in liquor as much as possible, and the aroma substance extracted from raw materials It cannot accurately restore the aroma concentration in liquor, so it is not conducive to professionals and ordinary consumers to more directly understand and define the "aroma substances" in liquor; When there are many aroma substances, some substances are low in content and cannot be collected; ③The collection of aroma substances in different time periods may cause the taste of some compounds with low threshold value to be masked by other tastes in this time period.

Therefore this area needs badly a kind of aroma solution preparation method that can accurately restore different flavors in liquor.

Contents of the invention

The technical problem to be solved by the invention is that the existing method for preparing the aroma solution in liquor cannot accurately restore the aroma of different flavors in the liquor.

The technical solution adopted by the present invention to solve the technical problem is: the preparation method of different aroma solutions in liquor, after taking the liquor and obtaining the concentrated solution through the steps of dilution, extraction and concentration, the concentrated solution is prepared by using a semi-preparative high performance liquid chromatograph Fractions containing different aromas were collected, and then the prepared different aroma substances were qualitatively and quantitatively analyzed by a olfactory instrument combined with a gas chromatography mass spectrometer, and finally aroma solutions were prepared according to the quantification to obtain different aroma solutions in liquor.

The above dilution is to take 10-50mL liquor sample and dilute it with saturated saline until the alcohol content is 1-10%.

The above extraction is to use ether-pentane solution to extract the diluted liquor sample three times, each time for 5-10 minutes.

Further, the volume ratio of ether to pentane in the ether-pentane solution is 1:1.

Further, the volume ratio of the ether-pentane solution to the diluted liquor sample is 3-4:6-7.

The above-mentioned concentration is to concentrate the extract by nitrogen blowing apparatus to obtain 0.5-1 mL of concentrated solution.

The specific method for preparing different aroma solutions in liquor is as follows: according to the content of different aroma substances in liquor, respectively dissolve different aroma substances in ethanol solutions with the same ethanol concentration as in the original liquor sample, and store in bottles.

The beneficial effects of the present invention are: the technical scheme of the present invention directly uses the concentrated liquor sample as the aroma extract, can separate as much as possible the different aroma substances in the liquor, qualitatively and quantitatively, and finally prepare different aroma solutions , the present invention more intuitively, concretely and accurately expresses the flavor characteristics of different types of liquor samples in different years.

A single aroma component cannot be well presented in liquor, and the method for preparing aroma in liquor in the prior art cannot restore aroma very well. The various aroma solutions prepared by the method of the present invention can make professional sensory evaluation personnel And ordinary consumers have a better understanding of the different aroma characteristics in liquor.

Description of drawings

Fig. 1 is the semi-preparation chromatogram of Wuliangye original wine sample of the embodiment of the present invention;

Fig. 2 is the gas chromatogram of fraction number F10 chocolate, nut aroma substance of the embodiment of the present invention;

Fig. 3 is the gas chromatogram of the marshmallow aroma substance of the fraction number F30 of the embodiment of the present invention.

Detailed ways

The technical solution of the present invention can be specifically implemented in the following manner.

The preparation method of different aroma solutions in white wine specifically comprises the following steps:

(1) Dilution: Take 10-50mL liquor sample and dilute it with saturated saline until the alcohol content is 1%-10%;

(2) Extraction: use ether-pentane (1: 1v/v) solution to extract the liquor sample three times, each extraction 5-10min, the volume ratio of the ether-pentane solution and the diluted liquor sample is 3- 4: 6-7.

(3) Concentration: Concentrate the extract with a nitrogen blower, and finally obtain a 0.5-1mL sample concentrate;

(4) Preparation: prepare the concentrated sample by using a semi-preparative high performance liquid chromatograph, and collect fractions containing different aromas;

(5) Qualitative: Qualitatively prepare different aroma substances by using a olfactory instrument in conjunction with a gas chromatography mass spectrometer;

(6) Quantification: accurately quantify the different aroma substances prepared by using a gas chromatography mass spectrometer;

(7) Preparation: According to the content of aroma substances in the white wine, different aroma substances are dissolved in ethanol solution (the concentration of the ethanol solution is the same as the concentration of ethanol in the liquor sample in step (1)), and bottled for preservation.

The technical solutions and effects of the present invention will be further described below through practical examples.

Example

The preparation method of different aroma solutions in white wine, the specific experimental steps are as follows:

(1) Take 50 mL of Wuliangye original wine with an alcohol content of 70%, and dilute it with saturated saline until the alcohol content is 10%, and the sample volume of the diluted original wine is 350 mL;

(2) Use ether-pentane (1:1 v/v) solution to extract the liquor sample three times (70, 70, 60 mL), the volume ratio of ether-pentane solution to the diluted liquor sample is 4:7, Extract 5 minutes each time, and obtain a total of 200 mL of extract;

(3) Concentrate the extract by nitrogen blowing apparatus, finally obtain 1mL sample concentrate;

(4) Prepare the concentrated sample by using a semi-preparative high-performance liquid chromatograph and collect fractions containing different aromas. The specific liquid chromatography condition parameters are as follows:

Chromatographic column: WatersAtlantis T3 OBD Prep (10mm×250mm×5μm); column temperature: 35°C; flow rate: 2mL/min; injection volume: 500μL; detector: DAD detector (220, 254nm); elution program: mobile phase A For water, mobile phase B is ethanol; 0min, A 100% 8min, A 80%; 28min, A 50%; 40min, A0%; 60min, A0%;

The semi-prepared chromatogram of the Wuliangye original wine sample in this example is shown in Figure 1. It can be seen from the figure that multiple chromatographic peaks appear under the elution of different proportions of the mobile phase, indicating that this method can directly separate the A variety of flavor substances, and by collecting fractions according to peaks, a total of 34 special fractions were finally collected, and the sensory evaluation was carried out by professional judges. The aroma description is shown in Table 1;

Table 134 Fraction Aroma Description

(5) Taking two of the special aromas (F10 and F30) as examples, the two aroma components were qualitatively characterized by a olfactory instrument combined with a gas chromatography-mass spectrometer (GC-O-MS), and the qualitative results are shown in Table 2 , the relevant condition parameters are as follows:

Capillary chromatographic column: HP-INNOWAX, 60m×0.32mm (inner diameter)×0.5μm (film thickness) or equivalent chromatographic column; inlet temperature: 240°C; /min increased to 240°C and kept for 15min; carrier gas: helium, purity ≧99.999%, flow rate 1mL/min; ionization mode: electron bombardment source (EI), energy 70eV; quadrupole temperature: 150°C; ion source temperature : 230°C; transfer line temperature: 250°C; timing event: 11.5min MS off, 15.0min MS on; sample injection mode: splitless mode; detection mode: full scan mode (SCAN); scan range: 35.00-350.00amu;

(6) The aroma components of F10 and F30 are further quantified by using gas chromatography mass spectrometry, 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): 60°C, equilibrate for 15min; 60°C, extract for 45min; 250°C, desorb for 3min.

Capillary chromatographic column: HP-INNOWAX, 60m×0.32mm (inner diameter)×0.5μm (film thickness) or equivalent chromatographic column; inlet temperature: 250°C; /min to 230°C for 10min; carrier gas: helium, purity ≧99.999%, flow rate 1mL/min; ionization mode: electron bombardment (EI), energy 70eV; quadrupole temperature: 150°C; ion source temperature : 230°C; transfer line temperature: 250°C; sample injection method: splitless mode; detection method: full scan mode (SCAN); scan range: 35.00-350.00amu;

Table 2 Qualitative and quantitative analysis results of aroma components of F10 and F30

The gas chromatogram of chocolate and nut aroma substances of fraction number F10 is shown in Figure 2; the gas chromatogram of fraction number F30 marshmallow aroma substances is shown in Figure 3;

(7) According to the measured content of F10 and F30 aroma substances in Wuliangye original liquor, these two aroma substances were dissolved in 70% ethanol solution respectively, bottled and preserved to obtain different aroma solutions in liquor.

It can be seen from the examples of the present invention that the method of the present invention can accurately prepare the solution of the aroma substances in the liquor, so as to present the flavor characteristics of the liquor more intuitively.

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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