CN110882289A - Method for preparing cocoa extract rich in cocoa polyphenol - Google Patents
Method for preparing cocoa extract rich in cocoa polyphenol Download PDFInfo
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- CN110882289A CN110882289A CN201911137689.1A CN201911137689A CN110882289A CN 110882289 A CN110882289 A CN 110882289A CN 201911137689 A CN201911137689 A CN 201911137689A CN 110882289 A CN110882289 A CN 110882289A
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- A61K36/00—Medicinal preparations of undetermined constitution containing material from algae, lichens, fungi or plants, or derivatives thereof, e.g. traditional herbal medicines
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
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- A61K2236/30—Extraction of the material
- A61K2236/33—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones
- A61K2236/333—Extraction of the material involving extraction with hydrophilic solvents, e.g. lower alcohols, esters or ketones using mixed solvents, e.g. 70% EtOH
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Abstract
The invention discloses a preparation method of a cocoa extract rich in cocoa polyphenol, which comprises the following processing steps: s1, squeezing the cocoa raw material to remove oil to obtain cocoa cake or cocoa powder; s2, extracting the cocoa cake or cocoa powder with normal hexane, and further removing grease; s3, immersing the cocoa cake or cocoa powder without oil and fat by taking an acetone-water solution as an extraction system for extraction, and decompressing the extraction solution to recover acetone; s4, adjusting the pH of the extracting solution after acetone recovery to 2.5-6, standing at normal temperature and filtering to obtain a precipitate and a filtrate; s5, washing the precipitate obtained in the S4 with a proper amount of water, and drying at low temperature and reduced pressure of 60 ℃ to obtain cocoa fat-soluble polyphenol; further drying the filtrate to obtain a non-fat soluble fraction; s6, mixing the cocoa fat-soluble polyphenol and the non-fat-soluble part in proportion to obtain the cocoa polyphenol with corresponding specification. The invention obtains the cocoa extract containing a large amount of polyphenols with high physiological activity by adjusting the proportion of the extraction solvent, the temperature and the pH value.
Description
Technical Field
The invention belongs to the technical field of cocoa extraction, and particularly relates to a preparation method of a cocoa extract rich in cocoa polyphenol.
Background
Cocoa (Theobroma cacao) is a small arbor of Theobroma of Sterculiaceae, and is widely cultivated in tropical regions of the world in the middle and south parts of America, and is cultivated in the southern China and the southern China. The seeds of cocoa are the main raw material for making cocoa powder and "chocolate candy". Is one of three major beverages in the world, and the main production areas are tropical areas such as Kotedawa, Venezuela, Brazil, Ganna, Peru, Indonesia and the like. Cocoa butter is the main flavor source of cocoa beans, and accounts for about 40-50% of the mass of cocoa beans. The components of cocoa beans remaining after removing cocoa butter and water are mainly starch, protein and fiber (30% -60%), and cocoa polyphenols account for about 8% -15%. The cocoa polyphenol has wide coverage, is one of the main active ingredients of cocoa products, and is a natural component with high safety.
The cocoa polyphenols mainly comprise flavonoid polyphenols and non-flavonoid polyphenols, and the flavonoid polyphenols mainly comprise Epicatechin (EC) and Catechin (-Catechin, C) monomers and polymers of the monomers; the non-flavonoid polyphenol mainly comprises monomers of phenolic acids such as Caffeic acid (Caffeic acid) and Chlorogenic acid (Chlorogenetic acid) and polymers of the monomers.
During the fermentation baking process after the collection of fresh cocoa beans, polyphenol oxidase (PPO) can promote the condensation of cocoa polyphenol. In order to inhibit the activity of PPO in cocoa products, special methods are needed to monitor the collection, pretreatment and extraction processes of cocoa beans. Because the cocoa seed treatment methods which can be collected in China are relatively consistent, the cost of the extraction process for inhibiting PPO activity and reducing polyphenol oxidation in the whole process is too high, and the operability is relatively low, a method for extracting cocoa polyphenol as far as possible under the condition that the quality of cocoa seeds and related raw materials is fixed is needed.
Disclosure of Invention
The present invention aims to provide a method for producing a cocoa extract rich in cocoa polyphenols, which can produce a cocoa extract containing a large amount of polyphenols with high physiological activities.
In order to achieve the purpose, the invention adopts the technical scheme that: a method for preparing cocoa extract rich in cocoa polyphenol comprises the following processing steps:
s1, squeezing the cocoa raw material to remove oil to obtain cocoa cake or cocoa powder;
s2, extracting the cocoa cake or cocoa powder with normal hexane, and further removing grease;
s3, immersing the cocoa cake or cocoa powder without oil and fat by taking an acetone-water solution as an extraction system for extraction, and decompressing the extraction solution to recover acetone;
s4, adjusting the pH of the extracting solution after acetone recovery to 2.5-6, standing at normal temperature and filtering to obtain a precipitate and a filtrate;
s5, washing the precipitate obtained in the S4 with a proper amount of water, and drying at low temperature and reduced pressure of 60 ℃ to obtain cocoa fat-soluble polyphenol; further drying the filtrate to obtain a non-fat soluble fraction;
s6, mixing the cocoa fat-soluble polyphenol and the non-fat-soluble part in proportion to obtain the cocoa polyphenol with corresponding specification.
The technical scheme of further improvement in the technical scheme is as follows:
1. in the scheme, the cocoa raw material in the step S1 is fermented or unfermented cocoa beans and/or cocoa shells, and the oil content of the pressed cocoa cakes or cocoa powder is 5-8%.
2. In the above scheme, the cocoa raw material pressing in step S1 requires that the temperature is controlled below 85 ℃, and the pressing into cocoa cake or cocoa powder is performed in an environment of more than 60 ℃ for no more than 3 minutes, so as to minimize the polymerization of polyphenol.
3. In the scheme, the material-liquid ratio of the cocoa cake or cocoa powder to the extracting solution in the step S2 is 1: 3-8.
4. In the above scheme, the fat content of the cocoa cake or cocoa powder further defatted in the step S2 is not more than 8 wt%.
5. In the scheme, the material-liquid ratio of the cocoa cake or cocoa powder to the extracting solution in the step S3 is 1: 4-20.
6. In the above scheme, the volume percentage of acetone in the acetone-water solution in step S3 is 30% to 90%.
7. In the scheme, the extraction temperature in the step S3 is 30-60 ℃, the extraction time is 30-120 minutes, and the temperature for recovering acetone under reduced pressure is 30-60 ℃.
8. In the above scheme, in step S4, inorganic acid is used to adjust the pH to 2.5-6.0, so that the solubility of alkaloid in cocoa can be enhanced, and after standing for 4-8 hours at normal temperature, filtering is performed to obtain a precipitate and a filtrate, wherein the precipitate is rich in fat-soluble polyphenol; the filtrate is rich in other non-fat soluble components, mainly alkaloids
9. In the above scheme, in the step S5, the content of cocoa fat-soluble polyphenols is calculated by a folin phenol-PC method, and the proportion of the total mass is not less than 30%.
10. In the above scheme, in the cocoa non-fat soluble fraction in step S5, the total alkaloid content is not less than 8%.
11. In the above embodiment, the mass mixing ratio of the cocoa polyphenol with the fat-soluble polyphenol and the non-fat-soluble fraction in the cocoa polyphenol with the corresponding specification in step S6 is 1: 0.1 to 20.
12. In the scheme, the total alkaloid content of the cocoa polyphenol is 0.1-20%, and the total polyphenol content is 10-60%.
Due to the application of the technical scheme, compared with the prior art, the invention has the following advantages:
1. the extraction process of the invention inhibits alcoholysis reaction in the extraction process of the traditional water-ethanol system to a great extent, the temperature of the system is lower, and the polyphenol structure in the raw material is kept as much as possible; in the final product, the total polyphenol content of the extract composition can be controlled at 10-60% and alkaloid content can be controlled at 0.1-20%.
2. The extraction process of the invention obtains the cocoa extract containing a large amount of polyphenols with high physiological activity by adjusting the proportion of the solvent for extraction, the temperature and the pH value.
Detailed Description
In the description of this patent, it is noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", etc., indicate orientations or positional relationships and are used merely to facilitate the description of the invention and to simplify the description, but do not indicate or imply that the device or element being referred to must have a particular orientation, be constructed and operated in a particular orientation, and therefore should not be construed as limiting the invention; the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance; furthermore, unless expressly stated or limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, as they may be fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; they may be connected directly or indirectly through intervening media, or they may be interconnected between two elements. The meaning of the above terms in this patent may be specifically understood by those of ordinary skill in the art.
The invention is further described below with reference to the following examples:
example 1:
100kg of cacao beans are squeezed to remove fat, and the cacao cake obtained after squeezing is subjected to reflux extraction with n-hexane at 60 ℃ for 1 hour. Filtering the cooled extractive solution. Extracting cocoa cake with 70% acetone-water solvent (800 kg) at 60 deg.C for 1 hr under reflux, recovering extractive solution at 55 deg.C under reduced pressure, concentrating to 200L, adding 0.1M hydrochloric acid solution, adjusting pH to 5.0, standing at room temperature for 8 hr, and filtering with plate and frame filter press. Drying the filtrate to obtain 11.38kg of non-fat soluble extract; filtering, washing with purified water, and drying at low temperature under reduced pressure of 60 deg.C to obtain cocoa fat soluble polyphenol 4.24 kg. Calculated by adopting a Folin phenol-PC method, the mass of polyphenol in cocoa fat-soluble polyphenol is 54 percent; the theobromine content in the non-fat soluble fraction extract was 11.2%.
Example 2:
1kg of defatted cocoa powder was placed in a flask and subjected to reflux extraction with 3L of n-hexane at 60 ℃ for 1 hour. Filtering the cooled extractive solution. Extracting cocoa powder with 10L 50% acetone-water solvent under reflux at 60 deg.C for 0.5 hr, filtering the extractive solution, recovering under reduced pressure at 60 deg.C in a rotary evaporation bottle of 20L, concentrating to 2L, adding 0.1M hydrochloric acid solution, adjusting pH to 3.5, standing at room temperature for 8 hr, and filtering. Drying the filtrate at 65 deg.C under reduced pressure to obtain 203g of non-fat soluble extract; and (3) washing the filtered precipitate with purified water, and drying at low temperature and reduced pressure of 60 ℃ to obtain 58g of cocoa fat-soluble polyphenol. Calculated by adopting a Folin phenol-PC method, the mass of polyphenol in cocoa fat-soluble polyphenol is 43 percent; the content of theobromine in the non-fat soluble fraction extract was 9.3%.
Example 3:
45.6kg of cacao beans were squeezed to remove fat, and the cacao cake obtained after squeezing was subjected to reflux extraction with n-hexane at 60 ℃ for 1 hour. Filtering the cooled extractive solution. Extracting cocoa cake with 90% acetone-water solvent (300 kg) at 55 deg.C for 2 hr under reflux, recovering extractive solution at 55 deg.C under reduced pressure, concentrating to 70L, adding 0.1M hydrochloric acid solution, adjusting pH to 3.0, standing at room temperature for 6 hr, and filtering with plate and frame filter press. Drying the filtrate to obtain 3.83kg of non-fat soluble extract; the filtrate is washed by purified water and dried under reduced pressure at 60 ℃ to obtain 2.34kg of cocoa fat-soluble polyphenol. Calculated by adopting a Folin phenol-PC method, the mass of polyphenol in cocoa fat-soluble polyphenol is 58 percent; the theobromine content in the non-fat soluble fraction extract was 8.4%. Mixing cocoa fat soluble polyphenol 2.0kg and non-fat soluble part 1.0kg to obtain cocoa extract with polyphenol content of 38%.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (10)
1. A method for preparing cocoa extract rich in cocoa polyphenol is characterized in that: the method comprises the following processing steps:
s1, squeezing the cocoa raw material to remove oil to obtain cocoa cake or cocoa powder;
s2, extracting the cocoa cake or cocoa powder with normal hexane, and further removing grease;
s3, immersing the cocoa cake or cocoa powder without oil and fat by taking an acetone-water solution as an extraction system for extraction, and decompressing the extraction solution to recover acetone;
s4, adjusting the pH of the extracting solution after acetone recovery to 2.5-6, standing at normal temperature and filtering to obtain a precipitate and a filtrate;
s5, washing the precipitate obtained in the S4 with a proper amount of water, and drying at low temperature and reduced pressure of 60 ℃ to obtain cocoa fat-soluble polyphenol; further drying the filtrate to obtain a non-fat soluble fraction;
s6, mixing the cocoa fat-soluble polyphenol and the non-fat-soluble part in proportion to obtain the cocoa polyphenol with corresponding specification.
2. The method of making a cocoa polyphenol rich cocoa extract as claimed in claim 1 wherein: in the step S1, the cocoa raw material is fermented or unfermented cocoa beans and/or cocoa shells, and the oil content of the pressed cocoa cakes or cocoa powder is 5-8%.
3. The method of making a cocoa polyphenol rich cocoa extract as claimed in claim 1 wherein: in the step S2, the ratio of the cocoa cake or cocoa powder to the extracting solution is 1: 3-8.
4. The method of making a cocoa polyphenol rich cocoa extract as claimed in claim 1 wherein: in the step S3, the ratio of the cocoa cake or cocoa powder to the extracting solution is 1: 4-20.
5. The method of making a cocoa polyphenol rich cocoa extract as claimed in claim 1 wherein: the volume percentage of acetone in the acetone-water solution in the step S3 is 30-90%.
6. The method of making a cocoa polyphenol rich cocoa extract as claimed in claim 1 wherein: in the step S3, the extraction temperature is 30-60 ℃, and the temperature for recovering acetone under reduced pressure is 30-60 ℃.
7. The method of making a cocoa polyphenol rich cocoa extract as claimed in claim 1 wherein: in the step S5, the content of cocoa fat-soluble polyphenol is calculated by a Folin phenol-PC method, and the proportion of the total mass is not less than 30%.
8. The method of making a cocoa polyphenol rich cocoa extract as claimed in claim 1 wherein: in the step S5, the proportion of the total weight of the cocoa non-fat soluble part and the alkaloid is not less than 8 percent.
9. The method of making a cocoa polyphenol rich cocoa extract as claimed in claim 1 wherein: in the cocoa polyphenol with the corresponding specification in the step S6, the mass mixing ratio of the cocoa fat-soluble polyphenol to the non-fat-soluble part is 1: 0.1 to 20.
10. The method of making a cocoa polyphenol rich cocoa extract as claimed in claim 1 wherein: the total alkaloid content of the cocoa polyphenol is 0.1-20%, and the total polyphenol content is 10-60%.
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872172A (en) * | 2005-05-31 | 2006-12-06 | 卡夫食品研发公司 | Polyphenol-enriched composition from cocoa shell extraction |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1872172A (en) * | 2005-05-31 | 2006-12-06 | 卡夫食品研发公司 | Polyphenol-enriched composition from cocoa shell extraction |
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