CN114540428B - Method for producing natural leaf alcohol by tea variable-temperature fermentation - Google Patents
Method for producing natural leaf alcohol by tea variable-temperature fermentation Download PDFInfo
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- CN114540428B CN114540428B CN202210233741.9A CN202210233741A CN114540428B CN 114540428 B CN114540428 B CN 114540428B CN 202210233741 A CN202210233741 A CN 202210233741A CN 114540428 B CN114540428 B CN 114540428B
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- C—CHEMISTRY; METALLURGY
- C12—BIOCHEMISTRY; BEER; SPIRITS; WINE; VINEGAR; MICROBIOLOGY; ENZYMOLOGY; MUTATION OR GENETIC ENGINEERING
- C12P—FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE
- C12P7/00—Preparation of oxygen-containing organic compounds
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- C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
- C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
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Abstract
The invention provides a method for producing natural leaf alcohol by tea variable-temperature fermentation, which comprises the following steps: s1: putting fresh tea leaves into a fermentation tank, adopting variable-temperature fermentation, and controlling the humidity to be 90% -100%; the temperature change range is 20 ℃ to 50 ℃ and the temperature rising speed is 0.8 ℃ to 1.2 ℃/h; after reaching 50 ℃, maintaining the temperature unchanged and continuing fermentation; the total fermentation time is controlled between 30 and 40 hours. According to the invention, the leaf alcohol content in the tea can be obviously improved by treating the tea in a variable-temperature fermentation mode, and the leaf alcohol content can be improved from 2% to more than 28%; compared with constant temperature fermentation, the method has very obvious improvement; the total yield of the post-treated phyllitol is more than 85%; is suitable for industrial production.
Description
Technical Field
The invention relates to the technical field of biosynthesis, in particular to a method for producing natural leaf alcohol by tea variable-temperature fermentation.
Background
Leaf alcohol, the chemical name cis-3-hexen-1-ol, is one of hexenol (hexenol), has green tender leaf fragrance, is clear, strong and natural, and has the fragrance, and at least 100 kinds of fragrances and essence contain leaf alcohol components, and the safe, nontoxic and side-effect-free leaf alcohol and its ester fragrances have become essential varieties in the fragrance industry.
The leaf alcohol can be used as a fragrant component in cosmetics, bath lotion, shampoo, cleaning agent, etc.; in addition, the beverage, cake, candy and the like using the edible essence can use the faint scent of the leaf alcohol and the fruit scent, so that the edible essence has certain development potential in the food industry; also in the case of insect attractants, is likewise a use of phyllitol.
Leaf alcohol is almost present in most green plants, but is mainly present in essential oils and fresh leaves of tea, peppermint, jasmine, grape, grapefruit, etc. Leaf alcohol is a food flavor which is allowed to be used in the standard regulation of GB2760-2014 in China, and can be added into soft drinks, cold drinks, candies and baked goods. However, natural leaf alcohol is produced only in india by esterifying the low boiling point fraction of waste peppermint oil with ethanol, separating leaf alcohol acetate, saponifying again to recover leaf alcohol, and finally separating to obtain 98% natural leaf alcohol. China is a large country for tea production, and has a large number of low-grade tea leaves which cannot be used as market products, and the tea leaves which are not fermented have low leaf alcohol content and cannot be directly extracted. Therefore, a method for producing natural phyllitol by variable-temperature fermentation is researched and developed, so that the natural phyllitol variety is also available in China.
Disclosure of Invention
The invention aims to provide a method for producing natural leaf alcohol by tea variable-temperature fermentation, which aims to solve the technical problems.
In order to achieve the above purpose, the method for producing natural leaf alcohol by tea variable-temperature fermentation comprises the following steps:
s1: putting fresh tea leaves into a fermentation tank, adopting variable-temperature fermentation, and controlling the humidity to be 90% -100%; the temperature change range is 20 ℃ to 50 ℃ and the temperature rising speed is 0.8 ℃ to 1.2 ℃/h; after reaching 50 ℃, maintaining the temperature unchanged and continuing fermentation; the total fermentation time is controlled to be 30-40 hours;
s2: distilling the fermented tea leaves by a steam distillation method; obtaining an aqueous solution containing leaf alcohol;
s3: extracting aqueous solution containing leaf alcohol with natural butanol, concentrating to obtain tea leaf oil containing leaf alcohol; rectifying the tea leaf oil containing the leaf alcohol to obtain the natural leaf alcohol.
Preferably, the humidity of the variable-temperature fermentation is controlled to be 92% -98%; the temperature rising speed of the variable-temperature fermentation is 1 ℃/h; the total fermentation time is controlled between 36 and 40 hours.
In addition, the raffinate obtained after the extraction of the natural butanol can be used as distilled water in a steam distillation method.
The beneficial effects are that: according to the invention, the leaf alcohol content in the tea can be obviously improved by treating the tea in a variable-temperature fermentation mode, and the leaf alcohol content can be improved from 2% to more than 28%; compared with constant temperature fermentation, the method has very obvious improvement; the total yield of the post-treated natural leaf alcohol is more than 85 percent; is suitable for industrial production.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is apparent that the described embodiments are some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention. Unless otherwise defined, technical or scientific terms used herein should be given the ordinary meaning as understood by one of ordinary skill in the art to which this invention belongs. As used herein, the word "comprising" and the like means that elements or items preceding the word are included in the element or item listed after the word and equivalents thereof without precluding other elements or items.
Aiming at the problems existing in the prior art, the embodiment of the invention provides a method for producing natural leaf alcohol by tea variable-temperature fermentation.
Example 1
Putting fresh tea leaves into a fermentation tank, and controlling the humidity to be 95%; adopting variable temperature fermentation, wherein the variable temperature range is 20-60 ℃ and the temperature rising speed is 1 ℃/h; sampling at 20 deg.C, 30 deg.C, 40 deg.C, 45 deg.C, 50 deg.C and 60 deg.C respectively, and distilling the samples by steam distillation; obtaining an aqueous solution containing leaf alcohol; extracting aqueous solution containing leaf alcohol by natural butanol, concentrating to obtain tea leaf oil containing leaf alcohol; detecting the leaf alcohol content of the tea leaf oil by a gas chromatography method;
the relationship between the leaf alcohol content and the gradual temperature rise is shown in Table 1.
TABLE 1
The results in Table 1 show that the content of leaf alcohol is continuously increased in the temperature range of 20-50 ℃ according to the temperature rising speed of 1 ℃/h during variable-temperature fermentation; at 40 ℃, the content of the leaf alcohol starts to be obviously increased, and at 50 ℃, the content of the leaf alcohol reaches the highest value; the reduction in leaf alcohol content occurs when the temperature reaches 60 c, presumably due to the fact that leaf alcohol volatilizes a part when the temperature is higher. Therefore, the proper temperature change range of the temperature change fermentation is finally determined to be 20-50 ℃.
Comparative example
Putting fresh tea leaves into a fermentation tank, and controlling the humidity to be 95%; fermenting at constant temperature at 20deg.C, 30deg.C, 40deg.C, 45deg.C, 50deg.C and 60deg.C for 40 hr, sampling after fermentation, and distilling the sample by steam distillation; obtaining an aqueous solution containing leaf alcohol; extracting aqueous solution containing leaf alcohol by natural butanol, concentrating to obtain tea leaf oil containing leaf alcohol; detecting the leaf alcohol content of the tea leaf oil by a gas chromatography method;
the relationship between the leaf alcohol content and the fixed temperature is shown in Table 2.
TABLE 2
The results in Table 2 show that the fermentation was carried out at a fixed temperature, and the leaf alcohol content was very low, and only 8% at 50℃and even at 60℃was reduced, probably due to volatilization of leaf alcohol.
By comparing the example 1 with the comparative example, it is found that the temperature swing fermentation has a significant increase in leaf alcohol content compared to the constant temperature fermentation.
Example 2
Putting fresh tea leaves into a fermentation tank, and controlling the humidity to be 95%; adopting variable temperature fermentation, wherein the variable temperature range is 20-50 ℃ and the temperature rising speed is 1 ℃/h; continuously maintaining the temperature of 50 ℃ for fermentation when the temperature reaches 50 ℃; the total fermentation time was 45 hours;
sampling at 15h, 20h, 25h, 30h, 35h, 40h and 45h respectively, and distilling the samples by a steam distillation method; obtaining an aqueous solution containing leaf alcohol; extracting aqueous solution containing leaf alcohol by natural butanol, concentrating to obtain tea leaf oil containing leaf alcohol; detecting the leaf alcohol content of the tea leaf oil by a gas chromatography method;
the relationship between leaf alcohol content and time is shown in Table 3.
TABLE 3 Table 3
The results in Table 3 show that the fermentation time reached 50℃at 30h, and the leaf alcohol content remained on an upward trend until 30h, and continued to ferment after reaching 50℃with a slight increase in leaf alcohol content, with very little increase in leaf alcohol content, reaching maximum at 40h, and remaining substantially unchanged at 45h and 40h. Thus, a suitable reaction time is 30 to 40 hours; more preferably from 36 to 40 hours.
Example 3
Putting fresh tea leaves into a fermentation tank, and fermenting at a variable temperature range of 20-50 ℃ at a heating rate of 1 ℃/h; continuously maintaining the temperature of 50 ℃ for fermentation when the temperature reaches 50 ℃; the total fermentation time was 40 hours; the humidity is controlled to be 30%, 50%, 70%, 90%, 95% and 100%, respectively; after fermentation, sampling is carried out respectively, and the samples are distilled by a steam distillation method; obtaining an aqueous solution containing leaf alcohol; extracting aqueous solution containing leaf alcohol by natural butanol, concentrating to obtain tea leaf oil containing leaf alcohol; detecting the leaf alcohol content of the tea leaf oil by a gas chromatography method;
the relationship between leaf alcohol content and humidity is shown in Table 4.
TABLE 4 Table 4
The results in table 4 show that: the humidity has a great influence on the content of leaf alcohol in the tea oil. Under the condition of low humidity, namely relatively dry, the content of the leaf alcohol is only 4 percent; after the humidity exceeds 90%, the content of the leaf alcohol is obviously improved, but the leaf alcohol has little change between 90% and 100%; thereby determining that the proper humidity is kept between 90% and 100%; more suitably 92-98%.
Example 4
S1, putting fresh tea leaves into a fermentation tank, and controlling the humidity to be 95%; adopting variable temperature fermentation, wherein the variable temperature range is 20-50 ℃, the temperature rising speed is 1 ℃/h, the temperature is maintained unchanged after the temperature reaches 50 ℃, and the continuous fermentation is maintained at 50 ℃; the total fermentation time is 38 hours;
s2, distilling the fermented tea leaves by a steam distillation method; obtaining an aqueous solution containing leaf alcohol;
s3: extracting aqueous solution containing leaf alcohol with natural butanol, concentrating to obtain tea leaf oil containing leaf alcohol; the content thereof was detected by gas chromatography to be 28.6%; rectifying the tea leaf oil containing the leaf alcohol to obtain natural leaf alcohol; the yield thereof was found to be 87%.
While embodiments of the present invention have been described in detail hereinabove, it will be apparent to those skilled in the art that various modifications and variations can be made to these embodiments. It is to be understood that such modifications and variations are within the scope and spirit of the present invention as set forth in the following claims. Moreover, the invention described herein is capable of other embodiments and of being practiced or of being carried out in various ways.
Claims (3)
1. A method for producing natural leaf alcohol by tea variable-temperature fermentation, which is characterized by comprising the following steps:
s1: fresh tea leaves are put into a fermentation tank, temperature-changing fermentation is adopted, the humidity is controlled to be 90% -100%, the temperature changing range is 20 ℃ -50 ℃, and the temperature rising speed is 0.8-1.2 ℃/h; after reaching 50 ℃, maintaining the temperature unchanged and continuing fermentation; the total fermentation time is controlled to be 30-40 hours;
s2: distilling the fermented tea leaves by a steam distillation method; obtaining an aqueous solution containing leaf alcohol;
s3: extracting aqueous solution containing leaf alcohol with natural butanol, concentrating to obtain tea leaf oil containing leaf alcohol; rectifying the tea leaf oil containing the leaf alcohol to obtain the natural leaf alcohol.
2. The method for producing natural leaf alcohol by variable temperature fermentation of tea leaves according to claim 1, wherein the humidity of the variable temperature fermentation is controlled to be 92% -98%; the temperature rising speed of the variable-temperature fermentation is 1 ℃/h; the total fermentation time is controlled between 36 and 40 hours.
3. The method for producing natural leaf alcohol by variable temperature fermentation of tea leaves according to claim 1, wherein raffinate obtained after extraction of natural butanol can be used as distilled water by steam distillation.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102771585A (en) * | 2012-08-17 | 2012-11-14 | 平月茶业（福建）有限公司 | Constant-humidity varying-temperature fermentation method for congou black tea |
| JP2015204754A (en) * | 2014-04-17 | 2015-11-19 | 長谷川香料株式会社 | Production method of green tea extract |
| CN109874883A (en) * | 2019-04-09 | 2019-06-14 | 重庆市农业科学院 | A kind of temperature-variable fermentation congou tea and its processing method |
| WO2020108956A1 (en) * | 2018-11-27 | 2020-06-04 | Unilever N.V. | A process of aroma recovery from tea leaf |
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- 2022-03-10 CN CN202210233741.9A patent/CN114540428B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102771585A (en) * | 2012-08-17 | 2012-11-14 | 平月茶业（福建）有限公司 | Constant-humidity varying-temperature fermentation method for congou black tea |
| JP2015204754A (en) * | 2014-04-17 | 2015-11-19 | 長谷川香料株式会社 | Production method of green tea extract |
| WO2020108956A1 (en) * | 2018-11-27 | 2020-06-04 | Unilever N.V. | A process of aroma recovery from tea leaf |
| CN109874883A (en) * | 2019-04-09 | 2019-06-14 | 重庆市农业科学院 | A kind of temperature-variable fermentation congou tea and its processing method |
Non-Patent Citations (2)
| Title |
|---|
| "New ethanol extraction improves the anti-obesity effects of black tea";Bongju Park et al.;《Arch Pharm Res》;第39卷(第3期);第310-320页 * |
| "茶叶挥发性成分中关键呈香成分研究进展";王梦琪 等;《食品科学》;第40卷(第23期);第341-349页 * |
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