CN110591825A - Preparation method of fenugreek concentrate - Google Patents
Preparation method of fenugreek concentrate Download PDFInfo
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- CN110591825A CN110591825A CN201911044744.2A CN201911044744A CN110591825A CN 110591825 A CN110591825 A CN 110591825A CN 201911044744 A CN201911044744 A CN 201911044744A CN 110591825 A CN110591825 A CN 110591825A
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- extraction
- fenugreek
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- ultrasonic
- fenugreek seeds
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/025—Recovery by solvent extraction
-
- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11B—PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES
- C11B9/00—Essential oils; Perfumes
- C11B9/02—Recovery or refining of essential oils from raw materials
- C11B9/027—Recovery of volatiles by distillation or stripping
Abstract
The invention relates to a preparation method of a fenugreek concentrate, which comprises the following steps of removing worm-eaten and mildewed fenugreek seeds, rotating at the temperature of 35-55 ℃ for 24-30 hours for germination, carrying out primary extraction by using an ethanol solution at the temperature of 21 ~ 25 ℃, carrying out re-extraction by using an ethanol solution at the temperature of 21 ~ 25 ℃ and concentrating at the vacuum degree of 0.090 ~ 0.098.098 MPa.
Description
Technical Field
The invention relates to a preparation method of a fenugreek concentrate, belonging to the technical field of extraction and separation methods of plant effective components.
Background
The fenugreek has specific fragrance, contains various fragrant substances such as fenugreek lactone, ionone, geranylacetone, linalool, ethyl myristate, ethyl caprylate, ethyl pentadecanoate and the like, and is a common high-quality raw material for preparing spices.
At present, most of the preparation methods of the fenugreek concentrate adopt the steps of baking and extracting the fenugreek, the concentrate prepared in the way mainly takes the scorched and sweet nut aroma and maple syrup-like aroma, but the low-boiling point or heat-sensitive aroma substances contained in the fenugreek are lost or damaged in the baking process, so that the aroma of the prepared fenugreek concentrate is not mellow and natural, and the aroma is single.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a manufacturing method of a fenugreek concentrate, the variety of aroma substances in the fenugreek concentrate prepared by the method is increased, and the content of the aroma substances is increased by more than 15%.
According to the technical scheme provided by the invention, the manufacturing method of the fenugreek concentrate comprises the following steps:
pretreatment: removing worm-eaten and mildewed fenugreek seeds;
germinating, namely filling the treated fenugreek seeds into a cylindrical container, adding deionized water which is 1.5-2.0 times of the weight of the fenugreek seeds into the container, rotating the container around the axis of the container, wherein the axis of the container is parallel to the horizontal plane, the rotating speed is 10 ~ 20 revolutions per minute, the temperature in the container is kept at 35-55 ℃, the rotating time is 24-30 hours, and the fenugreek seeds are subjected to primary germination in the container;
transferring the preliminarily germinated fenugreek seeds into an ultrasonic extractor, adding an ethanol solution which is 9 ~ 11 times of the weight of the fenugreek seeds into the ultrasonic extractor, wherein the concentration of the ethanol solution is 95 ~ 100% vol, carrying out ultrasonic extraction at 21 ~ 25 ℃ for 20 ~ 30 minutes, the stirring speed of a stirrer in the extraction period is 30 ~ 50 revolutions per minute during the ultrasonic extraction, discharging the primary extract after the extraction is finished, and leaving the fenugreek seeds;
adding an ethanol solution with the weight 3 ~ 6 times that of the fenugreek seeds into an ultrasonic extractor for re-extraction, wherein the concentration of the ethanol solution is 88 ~ 92% vol, carrying out ultrasonic extraction for 15 ~ 20 minutes at 21 ~ 25 ℃, the stirring speed of a stirrer during the ultrasonic extraction period is 30 ~ 50 revolutions per minute, and discharging re-extraction liquid after the extraction is finished;
concentrating the primary extract and the re-extract in a rotary evaporator under reduced pressure, wherein the vacuum degree of the rotary evaporator is 0.090 ~ 0.098Mpa, the material temperature is 55 ~ 60 deg.C, and the concentration is 30 ~ 50% of the weight of the raw materials, and the obtained concentrate is semen Trigonellae concentrate.
Preferably, in the preliminary extraction step, the power of the ultrasonic extractor is 600W ~ 1000W, and the frequency of the ultrasonic is 25 ~ 35 KHz.
Preferably, in the re-extraction step, the power of the ultrasonic extractor is 600W ~ 1000W, and the frequency of the ultrasonic is 25 ~ 35 KHz.
Preferably, the number of re-lifting is controlled to be 1 ~ 3 times.
The fenugreek concentrate obtained by the method has the advantages that the variety of aroma substances is increased, the content of the aroma substances is increased by more than 15%, and the product has unique aroma different from that of the traditional fenugreek concentrate, is weak in scorched aroma, prominent in sweet aroma and fruity aroma, and rich and various in aroma.
Detailed Description
The present invention will be further described with reference to the following specific examples.
The rotary evaporator used in the following examples was a RE-52AA rotary evaporator produced by Shanghai Yangrong Biochemical instruments works.
Example 1
A method for preparing fenugreek concentrate comprises the following steps;
pretreatment: removing worm-eaten and mildewed fenugreek seeds;
germination: loading the treated fenugreek seeds into a cylindrical container, adding deionized water which is 1.5 times of the weight of the fenugreek seeds into the container, enabling the container to rotate around the axis of the container, enabling the axis of the container to be parallel to a horizontal plane, enabling the rotation speed to be 10 revolutions per minute, keeping the temperature in the container at 35 ℃, and enabling the rotation time to be 30 hours, and enabling the fenugreek seeds to be subjected to primary germination in the container;
carrying out initial extraction: transferring the preliminarily germinated fenugreek seeds into an ultrasonic extractor, wherein the power of the ultrasonic extractor is 900W, the frequency of ultrasonic waves is 26KHz, adding an ethanol solution which is 9 times of the weight of the fenugreek seeds into the ultrasonic extractor, the concentration of the ethanol solution is 95% vol, carrying out ultrasonic extraction at 21 ℃ for 20 minutes, and when carrying out ultrasonic extraction, the stirring speed of a stirrer in an extraction period is 30 revolutions per minute, discharging an initial extract after the extraction is finished, and leaving the fenugreek seeds;
and then extracting: adding an ethanol solution 6 times the weight of the fenugreek seeds into an ultrasonic extractor for re-extraction, wherein the power of the ultrasonic extractor is 700W, the frequency of ultrasonic waves is 35KHz, the concentration of the ethanol solution is 92% vol, performing ultrasonic extraction for 15 minutes at 21 ℃, the stirring speed of a stirrer in the extraction period is 30 revolutions per minute during ultrasonic extraction, and discharging re-extraction solution after extraction is finished;
concentration: transferring the primary extract and the re-extract to a rotary evaporator for vacuum concentration, wherein the vacuum degree of the rotary evaporator is 0.090Mpa during concentration, the material temperature is 60 ℃, and the concentration is 30% of the weight of the input raw materials, and the obtained concentrate is the fenugreek concentrate.
Example 2
A method for preparing fenugreek concentrate comprises the following steps:
pretreatment: removing worm-eaten and mildewed fenugreek seeds;
germination: loading the treated fenugreek seeds into a cylindrical container, adding deionized water with the weight 2.0 times that of the fenugreek seeds into the container, enabling the container to rotate around the axis of the container, enabling the axis of the container to be parallel to the horizontal plane, enabling the rotation speed to be 20 revolutions per minute, keeping the temperature in the container at 55 ℃, and enabling the rotation time to be 24 hours, and enabling the fenugreek seeds to be subjected to primary germination in the container;
carrying out initial extraction: transferring the preliminarily germinated fenugreek seeds into an ultrasonic extractor, wherein the power of the ultrasonic extractor is 600W, the frequency of ultrasonic waves is 35KHz, adding an ethanol solution which is 11 times of the weight of the fenugreek seeds into the ultrasonic extractor, the concentration of the ethanol solution is 100% vol, carrying out ultrasonic extraction at 25 ℃ for 30 minutes, the stirring speed of a stirrer in the extraction period during the ultrasonic extraction is 50 revolutions per minute, discharging an initial extract after the extraction is finished, and leaving the fenugreek seeds;
and then extracting: adding an ethanol solution which is 3 times of the weight of the trigonella seed into an ultrasonic extractor for re-extraction, wherein the power of the ultrasonic extractor is 1000W, the frequency of ultrasonic waves is 25KHz, the concentration of the ethanol solution is 88% vol, performing ultrasonic extraction for 20 minutes at 25 ℃, the stirring speed of a stirrer in the extraction period is 50 revolutions per minute during ultrasonic extraction, repeating the re-extraction step for 2 times, repeating the re-extraction step for 1 time, and discharging re-extraction liquid after re-extraction is finished;
concentration: transferring the primary extract and the re-extract to a rotary evaporator, and concentrating under reduced pressure, wherein the vacuum degree of the rotary evaporator is 0.098Mpa, the material temperature is 55 ℃, and the concentration is 50% of the weight of the input raw materials, and the obtained concentrate is the fenugreek concentrate.
Example 3
A method for preparing fenugreek concentrate comprises the following steps:
pretreatment: removing worm-eaten and mildewed fenugreek seeds;
germination: loading the treated fenugreek seeds into a cylindrical container, adding deionized water which is 1.8 times of the weight of the fenugreek seeds into the container, enabling the container to rotate around the axis of the container, enabling the axis of the container to be parallel to the horizontal plane, enabling the rotation speed to be 15 revolutions per minute, keeping the temperature in the container at 45 ℃, and enabling the rotation time to be 27 hours, and enabling the fenugreek seeds to be subjected to primary germination in the container;
carrying out initial extraction: transferring the preliminarily germinated fenugreek seeds into an ultrasonic extractor, wherein the power of the ultrasonic extractor is 800W, the frequency of ultrasonic waves is 30KHz, adding an ethanol solution which is 10 times of the weight of the fenugreek seeds into the ultrasonic extractor, the concentration of the ethanol solution is 97% vol, carrying out ultrasonic extraction at 23 ℃ for 25 minutes, and discharging an initial extracting solution after the extraction at the stirring speed of 40 revolutions per minute during the extraction period of the ultrasonic extraction, so as to leave the fenugreek seeds;
and then extracting: adding an ethanol solution which is 4.5 times of the weight of the trigonella seed into an ultrasonic extractor for re-extraction, wherein the power of the ultrasonic extractor is 700W, the frequency of ultrasonic waves is 32KHz, the concentration of the ethanol solution is 90% vol, carrying out ultrasonic extraction for 17 minutes at 23 ℃, the stirring speed of a stirrer in the ultrasonic extraction period is 40 revolutions per minute, repeating the re-extraction step for 2 times, and discharging re-extraction liquid after re-extraction is finished;
concentration: transferring the primary extract and the re-extract to a rotary evaporator, and concentrating under reduced pressure, wherein the vacuum degree of the rotary evaporator is 0.094Mpa, the material temperature is 58 ℃, and the concentration is 45% of the weight of the input raw materials, and the obtained concentrate is the fenugreek concentrate.
The invention has the advantages that: the fenugreek seeds are properly germinated, biological enzymes in the seeds are activated, macromolecular substances are decomposed, various nutrient substances are provided for the biological activity of the seeds, and meanwhile, various new fragrant substances are generated, so that the types and the content of the fragrant substances are increased; meanwhile, the ultrasonic wave can break the shielding effect of cell wall breaking, is beneficial to the dissolution and diffusion of effective substances, improves the extraction effect, has short extraction time, has a protection effect on effective components which are unstable in heat and easy to hydrolyze or oxidize, increases the types of aroma substances in the concentrate, improves the content of the aroma substances by more than 15 percent, has more reasonable types and proportions of various aroma substances in the product, has different special aroma from the traditional fenugreek concentrate, has prominent sweet aroma and fruit aroma, is rich and diverse in aroma note, obviously improves the product quality, has mellow, natural, stable and lasting aroma, has good compatibility with various spices, and can be widely used for blending of middle-grade and high-grade essences.
Claims (4)
1. A method for preparing a fenugreek concentrate is characterized by comprising the following steps:
pretreatment: removing worm-eaten and mildewed fenugreek seeds;
germinating, namely filling the treated fenugreek seeds into a cylindrical container, adding deionized water which is 1.5-2.0 times of the weight of the fenugreek seeds into the container, rotating the container around the axis of the container, wherein the axis of the container is parallel to the horizontal plane, the rotating speed is 10 ~ 20 revolutions per minute, the temperature in the container is kept at 35-55 ℃, the rotating time is 24-30 hours, and the fenugreek seeds are subjected to primary germination in the container;
transferring the preliminarily germinated fenugreek seeds into an ultrasonic extractor, adding an ethanol solution which is 9 ~ 11 times of the weight of the fenugreek seeds into the ultrasonic extractor, wherein the concentration of the ethanol solution is 95 ~ 100% vol, carrying out ultrasonic extraction at 21 ~ 25 ℃ for 20 ~ 30 minutes, the stirring speed of a stirrer in the extraction period is 30 ~ 50 revolutions per minute during the ultrasonic extraction, discharging the primary extract after the extraction is finished, and leaving the fenugreek seeds;
adding an ethanol solution with the weight 3 ~ 6 times that of the fenugreek seeds into an ultrasonic extractor for re-extraction, wherein the concentration of the ethanol solution is 88 ~ 92% vol, carrying out ultrasonic extraction for 15 ~ 20 minutes at 21 ~ 25 ℃, the stirring speed of a stirrer during the ultrasonic extraction period is 30 ~ 50 revolutions per minute, and discharging re-extraction liquid after the extraction is finished;
concentrating the primary extract and the re-extract in a rotary evaporator under reduced pressure, wherein the vacuum degree of the rotary evaporator is 0.090 ~ 0.098Mpa, the material temperature is 55 ~ 60 deg.C, and the concentration is 30 ~ 50% of the weight of the raw materials, and the obtained concentrate is semen Trigonellae concentrate.
2. The method of claim 1, wherein the power of the ultrasonic extractor is 600W ~ 1000W, and the frequency of the ultrasonic is 25 ~ 35 KHz.
3. The method of claim 1, wherein the re-extraction step is performed at a frequency of 25 ~ 35KHz and a power of 600W ~ 1000W.
4. The method for producing fenugreek concentrate according to claim 1 or 3, wherein the number of re-extractions is controlled to 1 ~ 3 times.
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| CN201911044744.2A CN110591825A (en) | 2019-10-30 | 2019-10-30 | Preparation method of fenugreek concentrate |
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| CN201911044744.2A CN110591825A (en) | 2019-10-30 | 2019-10-30 | Preparation method of fenugreek concentrate |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102028734A (en) * | 2010-12-10 | 2011-04-27 | 湖北中烟工业有限责任公司 | Method for extracting flavone from fenugreek by microwave |
| CN102746410A (en) * | 2011-04-20 | 2012-10-24 | 成都华高药业有限公司 | Method for preparing high-content fenugreek gum |
| CN106190573A (en) * | 2016-07-20 | 2016-12-07 | 湖北中烟工业有限责任公司 | A kind of Semen Trigonellae enzymatic flavouring prepares method and the application thereof of volatile oil |
| CN106366207A (en) * | 2016-09-08 | 2017-02-01 | 天津现代职业技术学院 | Fenugreek water-soluble polysaccharide hand sanitizer and preparation method thereof |
| CN109331055A (en) * | 2018-09-17 | 2019-02-15 | 天津纳尔生物科技有限公司 | A kind of production method of fenugreek tincture |
-
2019
- 2019-10-30 CN CN201911044744.2A patent/CN110591825A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102028734A (en) * | 2010-12-10 | 2011-04-27 | 湖北中烟工业有限责任公司 | Method for extracting flavone from fenugreek by microwave |
| CN102746410A (en) * | 2011-04-20 | 2012-10-24 | 成都华高药业有限公司 | Method for preparing high-content fenugreek gum |
| CN106190573A (en) * | 2016-07-20 | 2016-12-07 | 湖北中烟工业有限责任公司 | A kind of Semen Trigonellae enzymatic flavouring prepares method and the application thereof of volatile oil |
| CN106366207A (en) * | 2016-09-08 | 2017-02-01 | 天津现代职业技术学院 | Fenugreek water-soluble polysaccharide hand sanitizer and preparation method thereof |
| CN109331055A (en) * | 2018-09-17 | 2019-02-15 | 天津纳尔生物科技有限公司 | A kind of production method of fenugreek tincture |
Non-Patent Citations (1)
| Title |
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| 张丽萍等编著: "《181种药用植物繁殖技术》", 31 July 2004, 中国农业出版社 * |
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Application publication date: 20191220 |
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