High-quality fruit distilled liquor and preparation method thereof

Abstract

The invention relates to the technical field of wine brewing, in particular to high-quality fruit distilled liquor and a preparation method thereof. The invention provides a preparation method of high-quality fruit distilled liquor, which comprises the following steps: adding fermented fruit liquor into a distillation kettle, distilling under the magnetic field intensity of 0-4.0 mT, condensing, and taking liquor to obtain the fruit distilled liquor. The method is used for preparing the fruit distilled liquor, so that the high-quality fruit distilled liquor is efficiently prepared. The method disclosed by the invention solves the problems that the distilled liquor prepared by tower type equipment is not rich in aroma substances, thin in taste and the like, realizes preparation of the high-quality fruit distilled liquor by the tower type distillation equipment, and is suitable for industrial popularization and application.

Description

Technical Field

[0001] The invention relates to the technical field of winemaking, and in particular to high-quality fruit distilled wine and a preparation method thereof. Background Art

[0002] The world's distilled spirits mainly include liquor, whiskey, brandy, vodka, rum, gin, etc. Charente pot stills, dregs stills, and Coffey (tower) stills are the most commonly used distillation equipment. Different distillation equipment has different production efficiency and flavor quality due to their different structures. The distillation of wine is not simply to obtain high-purity alcohol. The purpose of obtaining high-quality distilled wine is to obtain the key aroma components of distilled wine and reduce the content of undesirable substances.

[0003] The Charente distillation equipment was first used in the 8th century and was originally used for the distillation of spices. It was not until the 18th century that the equipment was modified and used for the distillation of brandy. During the distillation process of the Charente distillation unit, the alcohol vapor contacts the inner wall of the reflux retort and gooseneck tube of the distillation unit with a special shape, causing the vapor of the distillate to partially condense and reflux, thus forming a slight distillation effect. Practice has proved that compared with tower distillation, the brandy product obtained by pot distillation is richer in volatile flavor substances, so it is often used to prepare high-grade wines, but because the production requires two distillations, the industrialization efficiency is low and the investment in large-scale production is high.

[0004] The pomace distillation equipment is a special equipment for discontinuous or uninterrupted distillation of fruit distilled wine. It mainly supplies the pomace, wine mud and wine liquid after secondary fermentation of pomace after fermentation in the fruit wine factory. This equipment is a single distillation equipment, which can better retain the original fruit aroma. The equipment is easy to operate, has reliable performance and a high degree of automation. The quality of fruit wine distilled by this equipment is generally inferior to that of the Charente distillation equipment. Because this equipment does not require re-distillation, its distillation efficiency is higher than that of the Charente pot distillation equipment. The pomace distillation equipment can realize the distillation of solids, liquids and solid-liquid composites.

[0005] The tower distillation equipment originated from the distillation of alcohol. It is a typical distillation equipment that uses continuous feeding and uninterrupted alcohol thermal separation. Through direct heating, fractionation by multi-stage bubble tray fractionator, high-purity distilled alcohol of more than 80% (V / V) can be obtained at one time. Tower distillation equipment is widely used in the production of distilled liquor in the United States, India, Russia, the Philippines and other countries. Due to the high flavor requirements of fruit wine, the richness and coordination of product components are not as good as the above two equipment, but because this equipment has high heat exchange efficiency, energy saving and environmental protection, and convenient automatic control system, it is very suitable for the large-scale factory production of fruit distilled liquor. At present, the distilled liquor prepared by tower distillation has few types and low content of volatile aroma substances, and the prepared distilled liquor has problems such as insufficient aroma, poor typicality, and thin taste. Therefore, it is necessary to upgrade the tower distillation equipment, distill out the key good flavor substances in the wine as much as possible, and at the same time, reduce the distillation of bad flavor substances, and finally achieve the improvement of the quality of fruit distilled liquor prepared by tower distillation equipment.

[0006] Based on this, the present invention is proposed. Summary of the invention

[0007] The purpose of the present invention is to provide a method for preparing high-quality fruit distilled liquor.

[0008] In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions:

[0009] The present invention provides a method for preparing high-quality fruit distilled liquor, comprising the following steps:

[0010] The fermented fruit wine is added into a distillation kettle, distilled and condensed under a magnetic field strength of 0-4.0 mT, and the wine is taken to obtain the fruit distilled wine.

[0011] Preferably, the amount of fermented fruit wine added is 50% to 80% of the volume of the distillation kettle.

[0012] Preferably, the temperature in the kettle of the distillation tower is 75-98°C; the temperature at the top of the distillation tower is 65-96°C.

[0013] Preferably, the pressure inside the distillation tower is -0.05 to 0 MPa.

[0014] Preferably, the distillation tower has 25 to 30 plates.

[0015] The invention also provides a high-quality fruit distilled wine prepared by the preparation method.

[0016] Beneficial effects of the present invention:

[0017] The present invention adds fruit fermented wine into a distillation kettle, starts the magnet on the tower body and adjusts the magnetic field strength in time during the distillation process, performs distillation under the assistance of the magnetic field, cools, and takes the wine to prepare a high-quality fruit distilled wine. The method for preparing fruit distilled wine has a short time, simple operation, and high production efficiency, and the quality of the distilled wine is close to that of the distilled wine prepared by the Charente pot type equipment; the fruit distilled wine prepared by the method of the present invention is rich in flavor substances and their content, solves the problems of insufficient aroma, poor typicality, and thin taste of fruit distilled wine prepared by tower distillation equipment, realizes the preparation of high-quality fruit distilled wine prepared by tower distillation, and is suitable for industrial promotion and application.

[0018] The types of volatile substances in the fruit distilled wine prepared by the present invention are significantly increased compared with the types of volatile substances in the fruit distilled wine prepared by the traditional tower distillation method. Using apple as a raw material, when preparing apple distilled wine, the difference substances present are mainly 9-decenoic acid, methyl decanoate, α-farnesene, ethyl laurate and bellflower alcohol, etc., which mainly give the apple distilled wine produced by it a typical floral fragrance feature; in addition, the magnetic field-assisted tower distillation equipment is similar to the apple distilled wine prepared by the Charente pot distillation equipment, and both have a high content of β-damasconone, so that the prepared apple distilled wine has a strong rose aroma. The content is low in the apple distilled wine prepared by the peel residue distillation equipment, while the substance cannot be detected in the apple distilled wine prepared by the traditional tower distillation equipment. Therefore, the method of the present invention (magnetic field-assisted preparation of fruit distilled wine) can achieve the preparation of high-quality fruit distilled wine. BRIEF DESCRIPTION OF THE DRAWINGS

[0019] Figure 1 It is the determination result of methanol, higher alcohol, total acid and total ester;

[0020] Figure 2 This is the distribution map of volatile substances in apple distilled wine;

[0021] Figure 3 This is the distribution percentage of the relative content of volatile substances in apple distilled wine;

[0022] Figure 4 Heat map of cluster analysis of volatile substances in apple distilled wine;

[0023] Figure 5 The OPLS-DA model scores and permutation test diagrams of apple distilled wine, where A is the OPLS-DA score diagram (1 is magnetic field-assisted tower distillation, 2 is Charente pot distillation, 3 is skin and residue distillation, and 4 is tower distillation), and B is the OPLS-DA model permutation test diagram;

[0024] Figure 6The GC-IMS three-dimensional spectrum, two-dimensional top view spectrum and difference spectrum of apple distilled wine, among which A is the three-dimensional spectrum, B is the two-dimensional top view spectrum, C is the difference spectrum, Z represents tower distillation, H represents Charente pot distillation, T represents magnetic field-assisted tower distillation, and S represents skin and residue distillation;

[0025] Figure 7 The electronic nose radar chart and PCA chart of apple distilled wine obtained from apple distilled wine, where A is the radar chart and B is the PCA chart;

[0026] Figure 8 This is the sensory evaluation score chart of apple distilled liquor. DETAILED DESCRIPTION

[0027] The present invention provides a method for preparing high-quality fruit distilled liquor, comprising the following steps:

[0028] The fermented fruit wine is added into a distillation kettle, distilled and condensed under a magnetic field strength of 0-4.0 mT, and the wine is taken to obtain the fruit distilled wine.

[0029] In the present invention, the preparation method of the fermented fruit wine is as follows: active dry yeast is inoculated according to 0.2‰ of the mass of the juice, and fermented at 25°C until the residual total sugar is less than 0.5%, thereby obtaining the fermented fruit wine.

[0030] In the present invention, the magnetic field strength is preferably 2.5 to 3.5 mT, and more preferably 3 mT.

[0031] In the present invention, the added amount of the fermented fruit wine is 50% to 80% of the volume of the still, preferably 60% to 70% of the volume of the still, and more preferably 60% of the volume of the still.

[0032] In the present invention, the temperature in the kettle of the distillation tower is 75 to 98°C, preferably 75 to 96°C, and more preferably 86.5°C; the top temperature of the distillation tower is 65 to 96°C, preferably 75 to 86°C, and more preferably 78.5°C.

[0033] In the present invention, the pressure inside the distillation tower is -0.05 to 0 MPa, preferably -0.03 to 0.02 MPa, and more preferably -0.025 MPa.

[0034] In the present invention, the distillation tower has 25 to 30 plates, preferably 26 to 29 plates, and more preferably 28 plates.

[0035] The alcohol content of the fruit distilled liquor is ≥55% vol.

[0036] In the present invention, the condensation is performed step by step through tower plates.

[0037] The invention also provides a high-quality fruit distilled wine prepared by the preparation method.

[0038] The technical solutions provided by the present invention are described in detail below in conjunction with the embodiments, but they should not be construed as limiting the protection scope of the present invention.

[0039] Example 1 A method for preparing high-quality fruit distilled liquor

[0040] Apple fermented wine: inoculate active dry yeast at 0.2‰ of the mass of apple juice, and ferment at 25°C until the residual total sugar is less than 0.5% to obtain apple fermented wine.

[0041] The fermented apple wine is added into a still in an amount of 70% of the volume of the still. The number of plates of the distillation tower is 28. The temperature in the still is 86°C, the temperature at the top of the tower is 79°C, the pressure in the tower is -0.02MPa, and distillation is performed at a magnetic field strength of 2.0mT. The wine is condensed step by step through the tower plates, and the apple distilled wine with an alcohol content of more than 55%vol is collected to obtain the apple distilled wine.

[0042] The alcohol content is determined in accordance with GB 5009.225-2016 (“National Food Safety Standard - Determination of Ethanol Concentration in Wine” 2016).

[0043] Example 2 A method for preparing high-quality fruit distilled liquor

[0044] The preparation of apple fermented wine is as in Example 1;

[0045] The fermented apple wine is added into a distillation tower in an amount of 60% of the volume of the still. The distillation tower has 25 plates, the temperature in the still is 82°C, the temperature at the top of the tower is 75°C, the pressure in the tower is -0.03MPa, and distillation is performed at a magnetic field strength of 3.0mT. The wine is condensed step by step through the plates, and the apple distilled wine with an alcohol content of more than 55%vol is collected to obtain the apple distilled wine.

[0046] The alcohol content is determined in accordance with GB 5009.225-2016 (“National Food Safety Standard - Determination of Ethanol Concentration in Wine” 2016).

[0047] Example 3 A method for preparing high-quality fruit distilled liquor

[0048] The preparation of apple fermented wine is as in Example 1;

[0049] The fermented apple wine is added into a distillation tower in an amount of 80% of the volume of the still. The distillation tower has 27 plates, the temperature in the still is 80°C, the temperature at the top of the tower is 75°C, the pressure in the tower is -0.04MPa, and distillation is performed at a magnetic field strength of 4.0mT. The wine is condensed step by step through the plates, and the apple distilled wine with an alcohol content of more than 55%vol is collected to obtain the apple distilled wine.

[0050] The alcohol content is determined in accordance with GB 5009.225-2016 (“National Food Safety Standard - Determination of Ethanol Concentration in Wine” 2016).

[0051] Comparative Example 1 Charente Pot Distillation Equipment Distillation

[0052] The preparation of apple fermented wine is as in Example 1;

[0053] Pump the fermented apple wine into the Charente pot still in an amount of 70% of the volume of the still, perform a primary distillation to obtain crude distillate, add the crude distillate back into the Charente pot still for secondary distillation, collect apple distillate with an alcohol content of more than 55% vol, and obtain apple distillate.

[0054] The alcohol content is determined in accordance with GB 5009.225-2016 (“National Food Safety Standard - Determination of Ethanol Concentration in Wine” 2016).

[0055] Comparative Example 2 Tower distillation equipment distillation

[0056] Referring to Example 1, the difference from Example 1 is that no magnetic field is added, and the other steps are the same as Example 1.

[0057] Comparative Example 3: Distillation of skin residue distillation equipment

[0058] Pump the fermented apple wine into the still of the peel and residue distillation equipment, the added amount is 70% of the volume of the still, distillation is carried out by serial distillation, and the apple distilled wine with an alcohol content of more than 55% vol is collected to obtain the apple distilled wine.

[0059] The alcohol content is determined in accordance with GB 5009.225-2016 (“National Food Safety Standard - Determination of Ethanol Concentration in Wine” 2016).

[0060] Experimental Example 1

[0061] The apple fermented wine was distilled using the methods described in Example 1 (hereinafter referred to as magnetic field-assisted tower distillation) and Comparative Examples 1 to 3.

[0062] The time for distilling apple distilled wine by the distillation method described in Example 1 and Comparative Examples 1 to 3 was counted; the wine yield was calculated according to the following formula, and the results are shown in Table 1;

[0063] Wine yield (%, based on 40°) = (alcohol content of apple distilled wine / alcohol content of raw materials) × 100%;

[0064] Table 1 Yield and distillation time of apple distilled wine obtained by different distillation methods

[0065] Distillation method Distillation time / h Wine yield / % Magnetic Field Assisted Column Distillation 3 96.2 Charente pot still 24 89.8 Column distillation 3 96.3 Lecithin distillation 4 96.1

[0066] As can be seen from Table 1, the wine yields of magnetic field-assisted tower distillation, tower distillation and skin and residue distillation are close, all above 96%, while the wine yield of Charente pot distillation is relatively low. In addition, in terms of distillation time, Charente pot distillation takes the longest time, which is 24 hours; skin and residue distillation takes the second longest time, which is 4 hours; magnetic field-assisted tower distillation and tower distillation take the shortest time, both of which are 3 hours. Charente pot distillation takes a long time because after the first distillation of Charente pot distillation, the alcohol content of the distilled liquor is low, so the secondary distillation method is usually used to obtain high-alcohol liquor, which also takes a long time. The time required for magnetic field-assisted tower distillation and tower distillation is the same.

[0067] Experimental Example 2

[0068] The contents of methanol, higher alcohols, total acids and total esters in the apple distilled wines prepared by the distillation methods described in Example 1 and Comparative Examples 1 to 3 were measured. The results are as follows: Figure 1 As shown;

[0069] The methanol content is determined in accordance with GB 5009.266-2016 ("National Food Safety Standard Determination of Methanol in Foods" 2016); the contents of higher alcohols, total acids and total esters are determined in accordance with GB / T11856.2-2023 Quality Requirements for Spirits Part 2: Brandy.

[0070] Pectin is the basis for the production of methanol. During the fermentation and enzymatic hydrolysis process, pectin decomposes and produces methanol. Excessive methanol concentration will damage human nerves and cause harm to the drinker. Figure 1 It can be seen that there are significant differences in the methanol content of apple distilled wines produced by the four distillation methods. The methanol content produced by peel and residue distillation is the highest, which can reach 0.36g / L, and the methanol content produced by magnetic field-assisted tower distillation is the lowest, which is 0.20g / L.

[0071] Higher alcohols have a special aroma and are an important component of the aroma of distilled liquor. They can improve the typicality of the style of distilled liquor, but too high a content of higher alcohols can also cause damage to the human body and make people dizzy, nauseous and vomit. Figure 1 It can be seen that the higher alcohols produced by skin residue distillation and tower distillation are relatively high, 2.45g / L and 1.60g / L respectively; the higher alcohols produced by Charente pot distillation and magnetic field assisted tower distillation are both lower and close in content;

[0072] The total acid content of apple distilled wine will have a great impact on its taste and quality. Too high or too low total acid content will reduce its sensory quality. Too high total acid content will make the distilled wine taste sour and astringent, with poor coordination, affecting consumers' preferences. Too low total acid content will make the distilled wine taste less mellow and thin, lacking in layering and typical style. Therefore, the total acid content of distilled wine should be controlled to be moderate. A moderate total acid content can give the distilled wine a mellow taste and improve the layering of the distilled wine. Figure 1 It can be seen that the total acid content of apple distilled wine obtained by the four distillation methods is relatively suitable, and the total acid content of distilled wine obtained by Charente pot distillation and magnetic field-assisted tower distillation is relatively high;

[0073] The total ester content in apple distilled wine determines its aroma difference and is also one of the important indicators for judging the quality of distilled wine. Figure 1 It can be seen that the total ester content of apple distilled wine obtained by Charente pot still and magnetic field-assisted tower distillation is significantly higher than that of tower distillation and peel and residue distillation, which are 0.71g / L and 0.55g / L respectively, and the content of aroma substances is relatively high; the total ester content of apple distilled wine prepared by tower distillation equipment is the lowest, which is 0.15g / L, indicating that magnetic field assistance significantly increases the content of ester substances in the distilled wine, and the aroma is closer to the apple distilled wine prepared by Charente pot still.

[0074] Experimental Example 3

[0075] HS-SPME / GC-MS was used to analyze the types and proportions of volatile substances in the apple distilled wine obtained by the distillation method described in Example 1 and Comparative Examples 1 to 3. The results are shown in Figures 2 and Figures 2-3 As shown;

[0076] The specific steps of HS-SPME / GC-MS analysis are as follows:

[0077] Sample treatment: Take 1 mL of apple distilled wine, place 20 μL (40 μg / mL) of internal standard solution in a 20 mL headspace injection bottle, add 2 g of NaCl, cover and seal, and use it as the sample to be tested to complete the volatile substance detection; each group of samples was measured in parallel 3 times.

[0078] (1) Enrichment of aroma components

[0079] HS-SPME conditions: refer to the use of 50 / 30μm DVB / CAR / PDMS fiber extraction head for aroma enrichment, insert the aged solid phase microextraction head into the sample bottle, balance at 50℃ for 15min, push out the extraction head after equilibrium, enrich flavor substances under extraction and adsorption conditions for 30min, and perform GC-MS analysis;

[0080] (2) Detection of aroma components

[0081] GC conditions: DB-wax (30m×0.25mm×0.25μm) was used for gas chromatography; a constant flow of helium at 1mL / min was used to separate the derivatized substances, 1mL of sample was added to a 20mL headspace bottle, and the bottle was sealed with a cap; the injection port temperature was 260°C, and the temperature program was set at 40°C as the initial temperature for 5min, then increased to 220°C at a rate of 5°C / min, and then increased to 250°C at 20°C / min, and maintained for 2.5min;

[0082] MS conditions: ionization mode: electron ionization source, electron energy 70eV; interface temperature: 260℃; ion source temperature: 230℃; quadrupole temperature: 150℃; scanning mode: full scan; mass range: 20~400; NIST2017 spectral library;

[0083] (3) Qualitative and quantitative analysis of aroma components

[0084] Qualitative analysis: After the test is completed, the mass spectrum data and retention time of each volatile substance obtained are compared with the NIST2017 standard spectral library to qualitatively analyze the volatile substances; only the identification results with Qual>60 are reported;

[0085] Quantification: 2-octanol was selected as the internal standard substance, and quantification was performed by the internal standard method; the content of each volatile substance was calculated according to the peak area ratio of the volatile substance to the internal standard substance, and the calculation formula was as follows: concentration of volatile substance (μg / mL) = concentration of internal standard substance (μg / mL) / peak area of ​​internal standard substance × peak area of ​​volatile substance.

[0086] Table 2 Types and mass concentrations of volatile substances in apple distilled wine

[0087]

[0088]

[0089]

[0090]

[0091]

[0092]

[0093]

[0094] As shown in Table 2, a total of 73 substances were identified, of which 32 were common components. The 74 substances included 11 alcohols, 5 acids, 37 esters, 6 ketones, 5 aldehydes and 9 other substances. Among them, in terms of the types of volatile substances, the apple distilled wines obtained by the four distillation methods were significantly different. A total of 64 types of distilled wines produced by Charente pot distillation, 59 types of distilled wines produced by magnetic field-assisted tower distillation, 47 types of distilled wines produced by skin residue distillation, and 55 types of distilled wines produced by tower distillation were detected. It can be concluded that the types of volatile substances in distilled wines prepared by magnetic field-assisted tower distillation are higher than those prepared by tower distillation, indicating that the preparation of distilled wines by magnetic field-assisted tower equipment can increase the types of volatile substances in distilled wines.

[0095] Combination Figures 2-3 It can be seen that 10 alcohols, 4 acids, 30 esters, 5 ketones, 4 aldehydes and 6 other substances were detected in the apple distilled wine produced by magnetic field-assisted tower distillation. Among them, alcohols accounted for 12%, and trans-nerolidol had the aroma of roses and orange flowers. Acids accounted for 6%, mainly derived from fatty acid metabolism or the degradation of long-chain fatty acids. The main detected substances were lauric acid, 9-decenoic acid, and caproic acid. Among them, lauric acid has the smell of laurel oil, 9-decenoic acid has a fat smell accompanied by a waxy aroma, and caproic acid has a coconut oil smell. Esters accounted for 63%, which is the volatile substance with the highest content in the apple distilled wine produced by magnetic field-assisted tower distillation. It is a class of substances with aroma produced by esterification reaction of acids and alcohols. It is an important component of the aroma of distilled wine. The main detected substances are ethyl caprate, ethyl laurate, isopentyl caprate, etc. Among them, ethyl caprate has a fruity aroma, ethyl laurate has a fruity aroma accompanied by the scent of laurel, and isoamyl caprate has a rose aroma. Aldehydes and ketones are also important components of apple distilled wine, which contribute to the formation of the overall flavor of apple distilled wine. Ketones account for 4%, and the main detected substances are 2-pentadecanone, damascone, and methyl nonyl ketone. 2-pentadecanone has a fresh jasmine aroma, damascone has a strong rose aroma, and methyl nonyl ketone has a citrus aroma accompanied by oily smell. Aldehydes account for 9%, and the main detected substances are acetaldehyde and furfural. Acetaldehyde has a green leaf and grass smell, and furfural has a cinnamon oil aroma. Others such as 1,1-diethoxyethane and α-farnesene also play an important role in the aroma of distilled wine. 1,1-diethoxyethane has an aromatic smell, and α-farnesene has a fresh flower petal aroma. The joint participation of these substances forms the unique aroma and flavor of apple distilled wine.

[0096] In the apple distilled wine produced by Charente pot distillation, 8 kinds of alcohols, 4 kinds of acids, 35 kinds of esters, 5 kinds of ketones, 4 kinds of aldehydes and 8 kinds of other kinds were detected. Among them, alcohol substances accounted for 10%, and the main detected substances were n-octanol, phenylethanol and trans-nerolidol. N-octanol had a citrus aroma with oily smell, and phenylethanol had a rose aroma. Among them, the content of trans-nerolidol was higher than that of magnetic field-assisted tower distillation, which was 837.57μg / L. Acid substances accounted for 13%, and the main detected substances were myristic acid and lauric acid. Myristic acid had a pine camphor wood smell. The lauric acid content was significantly higher than the lauric acid content in the distilled wines produced by the other three distillation methods, which was 5289.2μg / L. Esters accounted for 66%, and the main detected substances were hexyl acetate, n-propyl propionate and ethyl laurate. Hexyl acetate had a fruity aroma, and n-propyl propionate had a pineapple wine smell. Compared with the other three distillation methods, octyl acetate and ethyl 7-octenoate are both ester substances unique to Charente pot distillation, with contents of 111.69μg / L and 14.63μg / L respectively. Octyl acetate has a floral and fruity aroma, while ethyl 7-octenoate has a rose aroma. Ketone substances account for 2%, and the main substances detected are 2-pentadecanone, damascone, and methyl nonyl ketone, and the contents are slightly lower than those of magnetic field-assisted tower distillation, and methyl nonyl ketone is only detected in magnetic field-assisted tower distillation and Charente pot distillation. Aldehyde substances account for 4%, and the main substances detected are acetaldehyde, hexanal and furfural, and the contents are also lower than those of magnetic field-assisted tower distillation. Other categories account for 4%, mainly α-farnesene and 1,1-diethoxyethane, with contents of 61.99μg / L and 1759.75μg / L respectively.

[0097] In the apple distilled wine made by peel residue distillation, 8 kinds of alcohols, 5 kinds of acids, 24 kinds of esters, 2 kinds of ketones, 3 kinds of aldehydes and 5 kinds of other kinds were detected. Among them, alcohols accounted for 14%, and the main detected substances were 1-nonanol, n-octanol and phenylethyl alcohol, among which 1-nonanol had a rose fragrance accompanied by oily wax. Acids accounted for 3%, and the main detected substances were caproic acid, lauric acid and acetic acid. Among them, acetic acid was a unique acid substance for peel residue distillation and had a vinegar taste. Esters accounted for 51%, and the main detected substances were n-butyl acetate and n-propyl propionate. Compared with the other three distillation methods, the contents of these two substances were the highest, and n-butyl acetate had a fruity aroma. Ketones accounted for 2%, and the main detected substances were geranyl acetone and 2-heptanone. Among them, 2-heptanone had a pear fragrance, and geranyl acetone was a unique ketone substance for peel residue distillation, with a floral aroma. Aldehydes accounted for 21%, and the main detected substances were acetaldehyde and hexanal. Other categories account for 8%, mainly 1,1-diethoxyethane and benzofuran. Benzofuran also contributes to the aroma of distilled liquor.

[0098] In the apple distilled wine produced by tower distillation, 10 alcohols, 3 acids, 31 esters, 3 ketones, 2 aldehydes and 6 other types were detected. Among them, alcohols accounted for 34%, and the main detected substances were bellflower alcohol and decanol. Acids accounted for 1%, and the main detected substances were 9-decenoic acid and myristic acid. Esters accounted for 46%, mainly ethyl decanoate and diisobutyl phthalate, and diisobutyl phthalate had a weak aroma. Compared with the other three distillation methods, the content of ethyl decanoate in apple distilled wine produced by tower distillation was the highest. Ketones accounted for 4%, and the main detected substances were 2-pentadecanone and damasconone. Aldehydes accounted for 1%, and the main detected substances were furfural and hexanal. Others accounted for 14%, mainly 1,1-diethoxyethane, iduran and benzyl methyl ether. Iduran had a rose scent, while benzyl methyl ether had a fruity and ylang-ylang scent.

[0099] From the above analysis, it can be concluded that both magnetic field-assisted tower distillation and Charente pot distillation have more ester substances and a higher proportion of ester substances, and the distilled liquors prepared by the two equipment are closer in the proportion of their components, which further confirms that the quality of the distilled liquor prepared by magnetic field-assisted tower distillation is closer to that of the distilled liquor prepared by Charente pot distillation.

[0100] Experimental Example 4

[0101] In order to further confirm the differences between the volatile substance samples of apple distilled wine obtained by different distillation methods, TBtools software was used to perform cluster analysis on the volatile substances in the apple distilled wines obtained by the methods described in Example 1 and Comparative Examples 1 to 3. The results are as follows: Figure 4 As shown;

[0102] It can be seen intuitively from the figure that the distilled spirits produced by magnetic field-assisted tower distillation and Charente pot distillation have more common volatile substances, and the aroma composition of the two is relatively similar.

[0103] Experimental Example 5

[0104] The simca software was used to perform orthogonal partial least squares discriminant analysis (OPLS-DA) on the aroma components of the apple distilled wine obtained by the distillation method described in Example 1 and Comparative Examples 1 to 3. The results are as follows: Figure 5 As shown;

[0105] OPLS-DA analysis is a supervised discriminant analysis statistical method. Through OPLS-DA, a relationship model between aroma substances and apple distilled wine sample categories is established to predict the categories of apple distilled wine samples, and then to compare the differences in aroma substances in apple distilled wines produced by different distillation methods; the fitting index of the model is obtained as follows: independent variable fitting index R 2 x=0.913, dependent variable fitting index R2 y=0.988, model prediction index Q 2 =0.936. 2 and Q 2 If the value exceeds 0.5, it means that the model fits well and has strong cumulative explanatory power and predictive power, and can well reduce the dimension of the data and make it visual. After 200 permutation tests, if Figure 5 As shown in B, R 2 =0.936, Q 2 =-0.281, all R 2 and Q 2 are lower than the original value, and Q 2 The negative value of the y-intercept indicates that the model prediction exponential type is not overfitting and the results are stable and reliable.

[0106] As can be seen from the figure, the samples of the four distillation methods are located in four different quadrants, which shows that the aroma substances of the apple distilled wines produced by the four distillation methods are significantly different. The greater the distance between the groups, the greater the difference in the aroma substance composition, and the closer the distance between the groups, the smaller the difference in the aroma substance composition. The apple distilled wines produced by peel and residue distillation and tower distillation are similar in aroma substance composition. The apple distilled wines produced by magnetic field-assisted tower distillation and Charente pot distillation are both on the right side of the coordinate axis, which further shows that the aroma substance composition of the distilled wines prepared by the two equipments is relatively close.

[0107] Experimental Example 6

[0108] The volatile substances of the apple distilled wine obtained by the distillation method described in Example 1 and Comparative Examples 1 to 3 were detected by GC-IMS technology, and the GC-IMS spectrum was prepared by using the Reporter plug-in. The results are as follows: Figure 6 As shown;

[0109] The specific detection methods are as follows:

[0110] (1) Sample preparation: 1 mL of apple distilled wine was placed in a 20 mL headspace injection bottle. Three parallel samples were set up in each group. The samples were injected after incubation at 500 rpm and 70 °C for 15 min.

[0111] (2) GC conditions

[0112] GC conditions: 0-2min drift gas is 150mL / min, carrier gas is 2mL / min; 2-10min drift gas is 150mL / min, carrier gas is increased from 2mL / min to 10mL / min; 10-30min drift gas is 150mL / min, carrier gas is increased from 10mL / min to 90mL / min; 30-40min drift gas is 150mL / min, carrier gas is 90mL / min.

[0113] (3) GC-IMS analysis conditions

[0114] GC-IMS analysis conditions: the chromatographic column model is MXT-WAX (30m×0.53mm, 1μm), the IMS temperature is set to 45℃, the chromatographic column temperature is set to 60℃, the injection needle temperature is set to 85℃, the carrier gas / drift gas is N2, the analysis time is 40min, and the automatic injection volume is 200μL.

[0115] Figure 6 A is the GC-IMS three-dimensional spectrum, which can intuitively show the differences in peak quantity and peak height between different samples. From the figure, it can be intuitively seen that the distribution of volatile substances in apple distilled wines produced by different distillation methods is similar, but the position and peak intensity have certain changes. In order to facilitate observation and comparison, dimensionality reduction processing was performed to obtain Figure 6 B GC-IMS two-dimensional top view spectrum, the horizontal axis is the normalized ion migration time, the thick red line at 1.0 on the horizontal axis is the reaction ion peak (RIP peak), and the vertical axis is the gas chromatography retention time. The positions and colors of the points formed by volatile substances in apple distilled wine obtained by different distillation methods are different, so the content and type of volatile substances are also different. The color of the point to the right of the red vertical line at 1.0 on the horizontal axis represents the content of volatile aroma components. The whiter the point, the lower the content, and the redder the point, the higher the content. The larger the point area, the higher the substance peak and the higher the substance content. Figure 6 As can be seen in B, the retention time of most signal peaks is 100-600s, and the migration time is in the region of 1.0-2.0ms. However, the retention time of individual volatile compound signal peaks is 800-1500s. This may be due to the low polarity of these compounds, which leads to a longer retention time of these volatile components in the non-polar column. Figure 6 A shows that the apple distillates obtained by magnetic field-assisted tower distillation and Charente pot distillation have rich types of volatile substances, while the apple distillates obtained by tower distillation and peel and residue distillation have fewer types of volatile substances, which is consistent with the conclusion drawn by HS-SPME / GC-MS, further confirming that magnetic field-assisted tower distillation can achieve the preparation of high-quality fruit distillates.

[0116] In order to more clearly compare the differences between the volatile substances of apple distilled wines produced by different distillation methods, the spectrum of tower distillation was used as a reference, and the spectra of Charente pot distillation, magnetic field-assisted tower distillation, and skin and residue distillation were used for reference subtraction. The obtained GC-IMS difference spectra are shown in the figure below. Figure 6As shown in C, if the content is similar, the color after subtraction is white, if the content is higher than the reference, the color after subtraction is red, and if the content is lower than the reference, the color after subtraction is blue. Through observation and comparison, it can be seen that there are more red spots in the subtraction spectra of Charente pot distillation and magnetic field-assisted tower distillation, while there are more blue spots in the subtraction spectra of skin and residue distillation, which further indicates that the apple distilled wine produced by Charente pot distillation and magnetic field-assisted tower distillation has a higher content of volatile substances.

[0117] Experimental Example 7

[0118] (1) An electronic nose was used to analyze the odor of the apple distilled wine obtained by the distillation method described in Example 1 and Comparative Examples 1 to 3. The results are as follows: Figure 7 As shown;

[0119] The specific detection steps are as follows:

[0120] Sample processing: 10 μL of apple distilled liquor was injected into a 10L gas sampling bag, filled with nitrogen, and equilibrated at room temperature for 5 minutes before electronic nose measurement;

[0121] The specific electronic nose parameter settings are as follows: cleaning time 300 s, zeroing time 5 s, preparation time 5 s, test time 120 s, internal flow rate 400 mL / min, and injection flow rate 100 mL / min.

[0122] from Figure 7 As can be seen from A, the response values ​​of apple distilled wines produced by different distillation methods on the 10 sensors are different. In general, the response values ​​of the electronic nose data on the five sensors W1S, W1W, W2S, W2W and W5S are higher than those on the other five sensors, and the response value of the W2S sensor is the highest. The response values ​​of the apple distilled wine produced by Charente pot distillation on the five sensors W1S, W1W, W2S, W2W and W5S are higher than those on the apple distilled wines produced by the other three distillation methods, indicating that the apple distilled wine produced by Charente pot distillation has a higher content of alcohols, aldehydes and ketones, aromatic substances, organic sulfides, methyl compounds, inorganic sulfides, terpenes and nitrogen oxides. On the two sensors W2S and W1W, the response value of magnetic field-assisted tower distillation is second only to that of Charente pot distillation, indicating that the content of alcohols, aldehydes and ketones, inorganic sulfides and nitrogen oxides in magnetic field-assisted tower distillation is also relatively rich.

[0123] The main volatile components in apple distilled wine are processed by dimensionality reduction to obtain its PCA diagram, as shown in Figure 7As shown in Figure B, the contribution rates of PC1 and PC2 are 73.3% and 24.0%, respectively, and the cumulative contribution rate is 97.3%, indicating that PC1 and PC2 can better reflect most of the information of the original data of the sample. The apple distilled wine produced by Charente pot distillation has an intersection with the Charente pot distillation, and the distance is relatively close, indicating that there are similar parts in the composition of volatile substances of the two; tower distillation is located in the second quadrant, which is far away from the other three distillation methods, indicating that there are large differences between it and other distillation methods. It can be seen that the aroma substance profile of Charente pot distillation is richer, followed by magnetic field-assisted tower distillation, which is consistent with the results obtained by the radar map of the electronic nose, further confirming that magnetic field-assisted tower distillation significantly improves the quality of fruit distilled wine prepared by the original tower distillation, and realizes the improvement of the flavor quality of fruit distilled wine.

[0124] (2) Refer to GB / T 11856.2-2023 Quality Requirements for Spirits Part 2: Evaluation Standards for Distilled Spirits and make some minor modifications. The sensory evaluation criteria are appearance, aroma, taste, and typicality. Appearance accounts for 20%, aroma accounts for 30%, taste accounts for 40%, and style evaluation accounts for 10%. The total score is 100 points, and the average score is taken as the final evaluation result. The specific standards are shown in Table 3;

[0125] Eight sensory assessors (4 males and 4 females, aged between 21 and 25 years old) with a professional background in food were used to conduct sensory evaluation. 10 mL of apple distilled wine was placed in a wine glass and randomly arranged for evaluation by the assessors. After each sample was evaluated, the mouth was rinsed with pure water. Each tasting interval was 5 minutes. The evaluation results are shown in the figure below. Figure 8 As shown;

[0126] Table 3 Scoring criteria for apple distilled wine

[0127]

[0128] Figure 8The sensory quality scores of apple distilled wines produced by four distillation methods are shown. From the total score, it can be seen that Charente pot distillation and magnetic field-assisted tower distillation have the highest comprehensive scores, followed by skin and dregs distillation, and tower distillation has the lowest comprehensive score, and there are differences among the four distillation methods. In terms of appearance, there is no significant difference in the scoring results of apple distilled wines produced by the four distillation methods (P>0.05), and Charente pot distillation and magnetic field-assisted tower distillation have the highest scores; in terms of aroma, the scores of apple distilled wines produced by Charente pot distillation and magnetic field-assisted tower distillation are significantly different from tower distillation and skin and dregs distillation (P<0.05), and magnetic field-assisted tower distillation has the highest score; in terms of taste, magnetic field-assisted tower distillation has the highest score, which is significantly different from tower distillation and skin and dregs distillation (P<0.05); in terms of typicality, Charente pot distillation has the highest score, with distinct distilled wine characteristics, and there is a significant difference between tower distillation and skin and dregs distillation (P<0.05).

[0129] It can be seen from the above embodiments that the present invention provides a high-quality fruit distilled liquor and a preparation method thereof, the distillation time of the method is short, the liquor yield is high, the operation is simple, and only one distillation is required to achieve a high alcohol content, and the production efficiency is high; the method of the present invention increases the content level of good flavor substances in the fruit distilled liquor, greatly improves the quality of the fruit distilled liquor, and is suitable for large-scale production.

[0130] The above is only a preferred embodiment of the present invention. It should be pointed out that for ordinary technicians in this technical field, several improvements and modifications can be made without departing from the principle of the present invention. These improvements and modifications should also be regarded as the scope of protection of the present invention.

Claims

1. A method for preparing high-quality fruit distilled liquor, characterized in that: The steps include: The fermented fruit wine is added into a distillation kettle, distilled and condensed under a magnetic field strength of 0-4.0 mT, and the wine is taken to obtain the fruit distilled wine.

2. The preparation method according to claim 1, characterized in that: The added amount of the fermented fruit wine is 50% to 80% of the volume of the distillation kettle.

3. The preparation method according to claim 2, characterized in that: The temperature in the kettle of the distillation tower is 75-98°C; the temperature at the top of the distillation tower is 65-96°C.

4. The preparation method according to claim 3, characterized in that: The internal pressure of the distillation tower is -0.05 to 0 MPa.

5. The preparation method according to claim 4, characterized in that: The distillation tower has 25 to 30 plates.

6. The preparation method according to any one of claims 1 to 5 produces a high-quality fruit distilled liquor.

Images