Citrus distilled liquor and preparation method thereof

Abstract

The invention discloses citrus distilled liquor and a preparation method thereof, and relates to the technical field of fruit liquor preparation. The citrus distilled liquor is prepared by the following steps: citrus treatment: selecting fresh and ripe citrus, peeling and crushing into fruit pulp, airing the citrus peel in the shade for later use, and adding pectinase into the fruit pulp to reduce viscosity; fermenting to produce wine: adjusting the sugar degree and pH of the fruit pulp, and inoculating saccharomyces cerevisiae for fermentation to obtain fermented raw wine; normal-pressure distillation: filling the fermented raw wine into a wine steamer, and performing normal-pressure distillation to obtain a wine body with the alcoholic strength of 22-28 degrees; performing reduced-pressure cross-steaming: loading the wine body obtained by the first distillation into a wine steamer, and performing reduced-pressure cross-steaming on the wine body and the dried orange peel in the shade to obtain base wine with the alcoholic strength of 38-45 degrees; and aging: storing the base wine in a shade place for 2-4 months to obtain a citrus distilled wine finished product. According to the method, debitterizing and deacidifying treatment does not need to be carried out on the wine making raw materials, seasoning and aroma increasing through soaking or adding other substances are not needed after distillation, and the prepared citrus distilled wine is clear, transparent and bright, prominent in citrus aroma and soft in taste and has a good market prospect.

Description

Technical Field

[0001] The present invention relates to the technical field of fruit wine making, and particularly relates to a citrus distilled wine and a preparation method thereof. Background Art

[0002] At present, the citrus planting area in China has exceeded 45 million mu, and the annual output has exceeded 60 million tons. Using citrus to make wine can solve problems such as fruit spoilage caused by overstock and the treatment of substandard fruits that do not meet the fruit grading standards due to external factors such as size, so as to reduce economic losses and increase the added value of citrus. Citrus wine is divided into two categories: fermented wine and distilled wine. Fermented wine is a low-alcohol fruit juice beverage formed by yeast fermentation of fruit juice after removing the peel or with the peel of citrus fruits. However, due to the higher content of bitter substances and organic acids in citrus than in other fruits, the bitterness of citrus fermented wine is prominent, the taste is hard, sour and astringent, and the irritation is strong, making it difficult to be accepted by consumers. In traditional citrus wine brewing, bitter inhibitors, adsorbents and debittering enzymes are usually added before or during fermentation, and chemical acid reduction is carried out using calcium carbonate, potassium bicarbonate, etc., or physical acid reduction is carried out by low-temperature freezing and adsorption methods. Patent CN117305042A adds a bacterial agent extract to the citrus juice after peeling and juicing, performs water bath debittering, then inoculates non-wine yeast for pre-fermentation, and further decomposes bitter substances and consumes organic acids by the action of microorganisms, and finally inoculates wine yeast for fermentation to produce wine. Citrus distilled wine is a high-alcohol beverage similar to white liquor obtained by distilling the above-mentioned fermented wine. Since the bitter substances in citrus (mainly flavonoids) generally exist in the form of aglycones and glycosides, their solubility and boiling point in water are relatively high, and only a small amount is distilled into the wine body. And the main organic acids contained in citrus (such as citric acid, malic acid, tartaric acid, etc.) have weaker volatility compared with esters and volatile oils with aromatic odors. Therefore, the bitterness and acidity of citrus distilled wine are both reduced, but the citrus flavor of the distilled wine is also greatly weakened. Patent CN102787043B ages the distilled citrus wine in an oak barrel for 1-3 years to prepare citrus brandy, and the oak barrel endows the wine body with aroma and improves the taste. Patent CN117305042A adds green tea water, concentrated citrus juice, aromatic extract, etc. to the citrus distilled wine for flavoring.

[0003] The above operations such as debittering, acid reduction and flavor enhancement after distillation undoubtedly increase the process and production cost of citrus wine making, and may also introduce some non-natural chemical components, and ultimately affect the aroma and taste of citrus wine. Therefore, it is still of important research and market value to develop a citrus wine with a simple production process, no addition and prominent orange flavor and its preparation method. Summary of the Invention

[0004] In order to simplify the technological process of making citrus wine and develop a citrus wine with prominent orange flavor and no additives, the present invention provides a citrus distilled wine and its preparation method, which does not require debittering and deacidifying treatment of the wine-making raw materials. After the citrus is peeled and crushed, the orange peel is cut into small pieces 3-5 cm in length, air-dried in the shade and reserved. The obtained pulp does not need solid-liquid separation. After adding pectinase for necessary viscosity reduction treatment, it is directly inoculated with acid- and bitterness-tolerant wine yeast for fermentation to produce wine. After fermentation, it is subjected to the first atmospheric distillation and the second vacuum serial distillation together with the air-dried orange peel, and then allowed to stand and age to obtain the citrus distilled wine. The citrus distilled wine prepared by the present invention is clear and bright, has a prominent orange flavor and a smooth taste. The specific technical scheme is as follows: (1) Citrus treatment: Peel fresh and ripe citrus, cut into pieces (in some cases, such as cutting the orange peel into small pieces 3-5 cm in length), air-dry in the shade at 10-20 °C for 6-8 days, and reserve; Take the peeled pulp and crush it into pulp, without solid-liquid separation, add pectinase with a final concentration of 40-60 mg / L to the pulp, and enzymatically hydrolyze at 45-50 °C for 4-6 hours.

[0005] (2) Fermentation to produce wine: Adjust the sugar content of the treated citrus pulp to 24-29 °Bx, adjust the pH to 3.5-5.5, then inoculate 1%-3% of the total mass of the wine yeast in the pulp, and ferment at a constant temperature of 24-32 °C, sealed and static for 6-8 days to obtain the original citrus fermented wine.

[0006] (3) Atmospheric distillation: Fill the original citrus fermented wine into a distiller, heat it to 90-95 °C under normal pressure, discard the first 2%-5% of the original fermented wine distilled (this part of the wine contains relatively more small-molecule volatile substances, such as methanol, formaldehyde, etc.), and stop distillation after collecting 25%-35% of the volume of the original fermented wine distilled later (at this time, most of the ethanol and aroma substances have been distilled out, and continuing distillation will increase the impurities that affect the quality of the wine, such as volatile acid substances in the distilled wine), to obtain the wine body of the first distillation.

[0007] (4) Vacuum serial distillation: Fill the wine body obtained from the first distillation into a cleaned distiller, place a stainless steel steamer 5-10 cm above the wine body in the distiller, evenly spread the air-dried orange peel over the entire steamer, use a vacuum pump to pump the absolute pressure in the distiller to 30-35 kPa, heat it to 45-55 °C, and maintain this condition for vacuum distillation. Stop distillation after collecting 25%-35% of the volume of the first distilled wine, to obtain the base wine of the citrus distilled wine.

[0008] (5) Aging: Fill the base wine of the citrus distilled wine into a stainless steel wine storage tank, seal it, and store it in the shade for 2-4 months to obtain the finished product of the citrus distilled wine.

[0009] In Step 1, the citrus is one or more of Satsuma mandarin, Fengnan mandarin, Guangxi sugar orange, Linhai mandarin, Hubei ponkan, and Jiangxi wogan, preferably Satsuma mandarin.

[0010] In Step 1, the pectinase is a solid pectinase purchased from Jiahe Xuri Company, with an enzyme activity of 30,000 u / g. There is no specific requirement for the type of pectinase used in the present invention, and the addition amount can be adjusted according to the activity of the purchased pectinase.

[0011] In Step 2, adjusting the sugar content of the citrus pulp means adding an appropriate amount of one of food-grade glucose, sucrose, and granulated sugar to the pulp whose viscosity has been reduced by pectinase, preferably food-grade glucose.

[0012] In Step 2, the Saccharomyces cerevisiae is one of the special yeast SY for wine and fruit wine purchased from Angel Yeast Company or the active dry yeast Vivance for wine, preferably yeast SY.

[0013] In Step 2, the alcohol content of the obtained original citrus fermented wine is 8 - 14 degrees, preferably the original fermented wine with an alcohol content of 12 degrees.

[0014] In Step 3, the alcohol content of the wine body obtained by the first distillation is 22 - 28 degrees, preferably 25 degrees.

[0015] In Step 4, the air-dried orange peel is obtained by air-drying in the shade all the peels produced from the raw material citrus used before brewing in this batch. The air-dried orange peel should evenly cover the entire steamer basket to prevent gaps that would cause the steam during wine steaming not to penetrate the orange peel. By selecting the size of the wine steamer or the steamer basket, the stacking thickness of the orange peel is 1.5 - 2.5 cm. If the orange peel layer is too thick, it will be difficult for the steam to penetrate the orange peel layer; if it is too thin, less terpene compounds will be carried out from the orange peel by the steam during reduced-pressure tandem steaming, and the orange fragrance will not be prominent.

[0016] In Step 4, the alcohol content of the base wine of the citrus distilled wine obtained by the second reduced-pressure tandem steaming is 38 - 45 degrees, preferably 42 degrees.

[0017] The present invention also provides a citrus distilled wine prepared by the described method. The content of terpene compounds in the citrus distilled wine reaches 860 - 890 mg / 100 mL, and it also includes a total ester content of 58 - 70 mg / 100 mL and a total acid content of 180 - 240 mg / 100 mL.

[0018] The beneficial effects of the present invention are as follows: (1) The preparation process of the citrus distilled liquor provided by the present invention is simple, and no other substances except the raw material citrus are added for flavor enhancement. Compared with the preparation methods of other citrus wines, the preparation method of the citrus distilled liquor provided by the present invention does not require debittering and deacidification treatment of the raw materials for liquor making. After the citrus is peeled, the fruit is crushed into pulp, and there is no need for solid-liquid separation. Only by referring to the brewing method of wine and adding pectinase to the pulp for viscosity reduction treatment. In the second distillation of the present invention, the peel of the citrus used as the raw material for liquor making in this batch is steam-distilled together with the wine body, endowing the wine body with citrus fragrance, and there is no need for other flavor enhancement treatments after distillation.

[0019] (2) In view of the fact that the bitter substances in citrus (mainly flavonoids) generally exist in the form of aglycones and glycosides, with high solubility and boiling point in water, and only a small amount is distilled into the wine body; the main organic acids contained in citrus (such as citric acid, malic acid, tartaric acid, etc.) have weaker volatility compared with esters and volatile oils with aromatic odors; the citrus peel contains richer volatile flavor substances (mainly terpene compounds), etc., the present invention provides a method of second-stage vacuum steam-distillation of the dried citrus peel together with the wine body obtained from the first-stage atmospheric distillation. Through a large number of experiments, it is found that when the alcohol content of the product citrus distilled liquor is controlled at 38-45 degrees, the wine body is clear and bright, with prominent orange fragrance and smooth taste, which not only endows the citrus distilled liquor with unique aroma and taste, but also conforms to the drinking habits of Chinese consumers. Specific embodiments

[0020] The following further explains the present invention in conjunction with embodiments. The following embodiments are only used to illustrate the present invention, but do not limit the scope of implementation of the present invention.

[0021] Example 1 The preparation method of citrus distilled liquor is as follows: (1) Citrus treatment: Peel fresh and mature Wenzhou mandarins (without size and fruit shape restrictions), and cut the citrus peel into small pieces of 3-5 cm, and air-dry them in the shade at 10-20 °C for 7 days for later use. Take the peeled pulp and use a juicer to crush it into pulp at high speed. There is no need for solid-liquid separation. Add pectinase with a final concentration of 50 mg / L to the pulp and enzymolyze it at 45 °C for 4 hours.

[0022] (2) Fermentation to produce liquor: Add food-grade glucose to adjust the sugar content of the pulp to 27 °Bx, adjust the pH to 4.5, and then inoculate 3% of the total mass of the pulp with the special wine yeast SY for wine and fruit wine purchased from Angel Yeast Co., Ltd. Ferment at a constant temperature of 28 °C, in a closed state and statically for 7 days to obtain the original citrus fermented wine.

[0023] (3) Atmospheric distillation: Fill the original citrus fermented wine into a distiller, control the heating temperature at 90 - 95 °C, and conduct atmospheric distillation. Discard the first 3% of the original fermented wine volume distilled out, which is the head wine. Stop distillation after collecting 30% of the original fermented wine volume distilled subsequently to obtain the body of the first distillation, with an alcohol content of 25 degrees.

[0024] (4) Vacuum tandem distillation: Fill the body obtained from the first distillation into a cleaned distiller. Place a stainless - steel steamer basket 5 cm above the body of the distiller. Evenly cover the entire steamer basket with air - dried orange peel. Use a vacuum pump to pump the absolute pressure in the distiller to 35 kpa, heat to 50 °C, and maintain this condition for vacuum distillation. Stop distillation after collecting 30% of the body of the first - distilled wine volume distilled out to obtain the base wine of the citrus distilled wine, with an alcohol content of 42 degrees.

[0025] (5) Aging: Fill the base wine of the citrus distilled wine into a stainless - steel wine storage tank, seal it, and store it in a cool place for 3 months to obtain the finished product of the citrus distilled wine.

[0026] Example 2 The method steps are the same as those in Example 1, except that in step (2), the special wine yeast SY for wine and fruit wine is replaced with the active dry wine yeast Vivance.

[0027] Comparative Example 1 Wine making by steaming without adding orange peel. The steps of citrus treatment, fermentation to produce wine, the first atmospheric distillation, and aging are the same as those in Example 1. Only when performing the second vacuum distillation, no orange peel is added. The specific operation is as follows: Fill the body obtained from the first distillation into a cleaned distiller. Use a vacuum pump to pump the absolute pressure in the distiller to 35 kpa, heat to 50 °C, and maintain this condition for vacuum distillation. Stop distillation after collecting 30% of the body of the first - distilled wine volume distilled out to obtain the base wine of the distilled wine without adding orange peel during steaming, with an alcohol content of 42 degrees. After aging by the same method as in Example 1, the citrus distilled wine without adding orange peel during steaming is obtained.

[0028] Comparative Example 2 Wine making by steaming orange peel under atmospheric pressure. The steps of citrus treatment, fermentation to produce wine, the first atmospheric distillation, and aging are the same as those in Example 1. Orange peel is added during the second distillation, but the distillation is carried out under atmospheric pressure. The specific operation is as follows: Put the liquor obtained from the first distillation into the cleaned distiller. Place a stainless-steel steamer basket 5 cm above the liquor in the distiller. Evenly spread the air-dried orange peels over the entire steamer basket. Control the heating temperature at 90 - 95 °C and conduct atmospheric distillation. Stop distillation after collecting 30% of the volume of the liquor distilled out for the first time to obtain the base liquor of the orange peel atmospheric infusion-distilled liquor, with an alcohol content of 42 degrees. After aging in the same method as in Example 1, the orange peel atmospheric infusion-distilled orange liquor is obtained.

[0029] The sensory evaluation results of the orange liquors prepared in Example 1, Example 2, Comparative Example 1, and Comparative Example 2 are shown in Table 1. The alcohol content of these 4 products is 42 degrees, and the liquor bodies are all colorless, clear, and transparent, which are the results obtained through multiple experiments. It was found in the research that when the alcohol content of the orange liquor > 38 degrees, the liquor body is clear and transparent, without suspension or insoluble substances, and does not require filtration or clarification treatment. When the alcohol content is 42 degrees, the aroma and taste are the best. The orange liquors prepared in Example 1 and Example 2 have prominent orange flavors, rich aromas, full and rich tastes, with an obvious orange flavor when entering the mouth, and the aftertaste has a certain flavor of light-flavor Baijiu. In the product of Comparative Example 1, since there is no orange peel infusion-distillation during preparation, the orange flavor of the liquor body theoretically only comes from the original orange fermentation liquor, so the orange flavor is not prominent, and the taste is light and slightly bitter. In the product of Comparative Example 2, because the orange peel atmospheric infusion-distillation method is used during preparation, the temperature during the second distillation is 90 - 95 °C, and because the distillation time is relatively long, the obtained orange liquor product contains a special cooked orange peel flavor, which masks the unique freshness of the orange and affects the taste of the liquor body.

[0030] Table 1: Example 1, Example 2, Comparative Example 1, and Comparative Example 2 Sensory evaluation results of the orange liquor products prepared

[0031] The detection results of the main components and their contents that affect the aroma and taste of the orange liquor products prepared in Example 1, Example 2, Comparative Example 1, and Comparative Example 2 are shown in Table 2. It should be noted that this invention is obtained on the basis of multiple experiments, so the content determination results are expressed in the form of a range. According to relevant literature reports, among them, the detection of terpene compounds and total esters uses gas chromatography-mass spectrometry (GC-MS) method, and the detection of total acids and flavonoids uses high-performance liquid chromatography-mass spectrometry (HPLC-MS) method.

[0032] The content of terpenoid compounds in the citrus distilled liquor prepared in Example 1 is close to 900 mg / 100 mL (the three terpenoid compounds with the highest content are D-limonene, γ-terpinene, and β-myrcene), which is much higher than the content of esters and total acids, the main flavor substances in traditional Chinese liquor. The content of flavonoid substances that cause the bitterness of citrus liquor is only 17-21 mg / 100 mL. Therefore, this product has a prominent orange flavor, forming a unique aroma and taste. In the product of Comparative Example 1, since there is no co-steaming with orange peel during preparation, the terpenoid compounds theoretically only come from the distillation of the fermented liquor brewed from citrus fruits. Although terpenoid compounds are highly volatile, the content of terpenoid compounds in orange peel is much higher than that in fruits, and the types of terpenoid compounds contained are also different. Therefore, the content of terpenoid compounds in the product of Comparative Example 1 is <180 mg / 100 mL, and the three terpenoid compounds with the highest content are (+)-dipentene, γ-terpinene, and 2-carene. The main ester substances in the citrus distilled liquor products prepared in Example 1, Comparative Example 1, and Comparative Example 2 are ethyl acetate, ethyl lactate, and ethyl caprylate. Among them, ethyl acetate and ethyl lactate are the main flavor substances of light-flavor Chinese liquor. Therefore, the product of Example 1 has a certain light-flavor Chinese liquor flavor when it returns a sweet taste. Ethyl acetate and ethyl lactate are mainly produced by Saccharomyces cerevisiae during fermentation, and ethyl caprylate may mainly come from citrus. The main acid substances in the product are all lactic acid, acetic acid, and malic acid. The contents of these 3 acids in citrus fruits are relatively high themselves, and Saccharomyces cerevisiae will also produce a certain amount of lactic acid and acetic acid during fermentation. Literature reports that the largest organic acid in citrus is citric acid, but the content of citric acid in citrus distilled liquor is relatively low, which may be due to the utilization of citric acid by microorganisms during the brewing process or the thermal decomposition during distillation, which is beneficial to the acid reduction of citrus distilled liquor. In the product of Comparative Example 2, since the co-steaming of orange peel under normal pressure was adopted during preparation, and the temperature during the second distillation was 90-95 °C, compared with the vacuum co-steaming (50 °C) in Example 1, the distillation was more complete, and the contents of terpenoid compounds, total esters, and total acids all increased. However, the product of Comparative Example 2 has the taste of cooked orange peel, which affects the aroma and taste of the wine body. The main components (reasons) causing the taste of cooked orange peel could not be measured by GC-MS and HPLC-MS, but it can be avoided by vacuum co-steaming. Different yeasts were used in the brewing process of the wine bodies in Example 1 and Example 2. Compared with Example 1, the total ester and total acid contents of the product of Example 2 are slightly lower, but the types are basically the same. This shows that the yeast Vivance used in Example 2 has a stronger ability to decompose and transform organic acids in the raw materials than the yeast SY used in Example 1, but a relatively weaker ability to synthesize ester substances. Therefore, the product quality of Example 1 is better than that of Example 2, but there is no obvious difference in their sensory evaluation results. Comparing the products of Example 1 and Comparative Example 1, it was found that co-steaming with orange peel is beneficial to reducing the contents of polar substances such as total acid and formaldehyde in the finished product.Orange peel itself has a large number of micropores and is often used to adsorb odors. After being dried in the shade, hydrogen bonds are easily formed between the orange peel and the wine body during co-steaming after the surface bound water, so some polar substances such as organic acids or aldehydes can be adsorbed during co-steaming. Formaldehyde is likely to accumulate during the distillation of white wine, while the method of co-steaming with orange peel provided by the present invention reduces the formaldehyde content in the product by more than 50%.

[0033] Table 2: Detection results of the main components and contents affecting the aroma and taste of the citrus distilled wine products prepared in Example 1, Example 2, Comparative Example 1 and Comparative Example 2 (unit: mg / 100 mL)

Claims

1. A method for preparing citrus distilled liquor, characterized in that: The steps include: (1) Citrus processing: peel fresh and ripe citrus, cut into pieces, and air-dry in a cool place at 10-20°C for 6-8 days for later use; crush the peeled pulp into pulp, and add pectinase to the pulp for enzymatic hydrolysis and viscosity reduction; (2) Fermentation to produce wine: inoculating the enzymatically hydrolyzed citrus pulp with brewer's yeast, and fermenting it at a constant temperature of 24-32° C. in a sealed manner for 6-8 days to obtain citrus fermented raw wine; (3) atmospheric pressure distillation: heating the citrus fermented wine to 90-95° C. under atmospheric pressure for the first distillation, discarding the head wine, and collecting the distilled wine to obtain the first distilled wine; (4) vacuum distillation: the wine obtained by the first distillation is vacuumized and then heated to 45-55° C. for vacuum distillation. During the distillation process, shade-dried orange peels are placed above the wine so that steam can penetrate the orange peels during distillation to obtain a base wine of citrus distilled wine; (5) Aging: The base wine of the citrus distilled wine is placed in a wine storage container, sealed, and stored in a cool place for 2-4 months to obtain a finished citrus distilled wine.

2. The method for preparing citrus distilled liquor according to claim 1, characterized in that: The citrus includes one or more of Wenzhou mandarin orange, Fengnan mandarin orange, Guangxi sugar orange, Linhai mandarin orange, Hubei mandarin orange and Jiangxi Wogan orange.

3. The method for preparing citrus distilled liquor according to claim 1, characterized in that: In the step (2), the sugar content of the citrus pulp is adjusted to 24-29° Bx and the pH is adjusted to 3.5-5.5 before inoculating the citrus pulp with brewer's yeast.

4. The method for preparing citrus distilled liquor according to claim 1, characterized in that: In the step (2), the brewing yeast is the wine active dry yeast Vivance or the wine and fruit wine yeast SY purchased from Angel Yeast Company.

5. The method for preparing citrus distilled liquor according to claim 1, characterized in that: In the step (2), the alcohol content of the fermented citrus wine obtained is 8-14 degrees, preferably 12 degrees.

6. The method for preparing citrus distilled liquor according to claim 1, characterized in that: In the step (3), during the first distillation, 2%-5% of the volume of the fermented liquor initially distilled is discarded, and 25%-35% of the volume of the fermented liquor subsequently distilled is collected and then the distillation is stopped to serve as the liquor for the first distillation.

7. The method for preparing citrus distilled liquor according to claim 6, characterized in that: In the step (3), the alcohol content of the wine obtained by the first distillation is 22-28 degrees, preferably 25 degrees.

8. The method for preparing citrus distilled liquor according to claim 1, characterized in that: In the step (4), the vacuum pump is pumped to 30-35 kPa, heated to 50-55°C for reduced pressure distillation, and the distillation is stopped after collecting 25%-35% of the volume of the first distilled liquor to obtain the base liquor of citrus distilled liquor.

9. The method for preparing citrus distilled liquor according to claim 8, characterized in that: In the step (4), the alcohol content of the base liquor of the citrus distilled liquor obtained by the second reduced pressure distillation is 38-45 degrees, preferably 42 degrees.

10. A citrus distilled liquor, characterized in that: The citrus distilled liquor is prepared by the method described in any one of claims 1 to 9, and the terpene compound content of the citrus distilled liquor reaches 860-890 mg / 100mL.

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