CN101638366A - Method for extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux - Google Patents
Method for extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux Download PDFInfo
- Publication number
- CN101638366A CN101638366A CN200910184594A CN200910184594A CN101638366A CN 101638366 A CN101638366 A CN 101638366A CN 200910184594 A CN200910184594 A CN 200910184594A CN 200910184594 A CN200910184594 A CN 200910184594A CN 101638366 A CN101638366 A CN 101638366A
- Authority
- CN
- China
- Prior art keywords
- chlorogenic acid
- microwave
- extraction
- sunflower seed
- extracting
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
Images
Landscapes
- Coloring Foods And Improving Nutritive Qualities (AREA)
- Extraction Or Liquid Replacement (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a method for extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux, belonging to the field of biological engineering. The method comprises the following steps: crushing the sunflower seed dregs into 20-100 meshes; adding 30-70 percent of alcohol aqueous solution, wherein the extraction solid-liquid ratio is the quality-to-volume ratio of 1:6-1:18; extracting chlorogenic acid by the auxiliary reflux at a microwave frequency of 2450MHz and the microwave extraction power of 200-700w for 20-60 minutes; filtering extraction liquid with a bag-typecentrifuger after extraction is finished; concentrating filter liquid in vacuum under a vacuum degree of 0.05-0.095MPa at 60 DEG C until the concentration of dry substances is 30 percent by mass; andspraying and drying to obtain a chlorogenic acid product. The invention adopts the method for extracting the chlorogenic acid of the sunflower seed dregs by the microwave auxiliary reflux, has continuously acting microwaves in the extraction process, short extraction time, high efficiency and small solvent consumption and improves the chlorogenic acid yield of the product by 1.54-2.39 times thanthat of a traditional alcohol solvent extraction method.
Description
Technical field:
The present invention relates to bioengineering field, be specifically related to the protective foods production technology, refering in particular to the sunflower seed dregs is raw material, utilizes the microwave auxiliary reflux extractive technique to prepare the method for chlorogenic acid.
Background technology:
Sunflower seed dregs is nutritious, and output occupies second in all oil meal classes of the world, be often used as feed, but the easy oxidized formation o-quinone of its contained chlorogenic acid and generate the non-nutritive ingredient that non-ruminant animal can't digest with protein molecule reaction.Chlorogenic acid is a kind of effective phenolic antioxidant, also antibiotic, antiviral, the leukocyte increasing of tool, hemostasis, hepatic cholagogic, hypotensive, promote effects such as enterogastric peristalsis, antitumor, lipopenicillinase, removing free radical.The content of chlorogenic acid in sunflower seed dregs reaches 1.5% to 3%, chlorogenic acid if can be extracted, not only can obtain enormous amount, have the chlorogenic acid product of higher resistance of oxidation or pharmaceutical use, also can eliminate the antinutritional factor of sunflower seed dregs, be the condition of having created of further utilizing.
Extracting method to chlorogenic acid in sunflower seeds, the sunflower meal mainly contains at present: the patent of ZL 200510047693.0 adopts the alcohol solvent circumfluence method to extract chlorogenic acid in the sunflower meal, the patent of ZL 200510094347.8 adopts macroporous resin adsorption to separate chlorogenic acid in the sunflower cake, and application number is that 200810109773.8 patent adopts ethanol water diacolation method to extract chlorogenic acid in the certain herbaceous plants with big flowers dregs of rice.These method ubiquity operation steps complexity, extraction time are grown, solvent load is big or extract shortcomings such as yield is low.
Microwave-assisted extracts that (Microwave-assisted Extraction MAE) is the new technology that a kind of recent development of utilizing micro-wave energy to improve extraction yield is got up.Its ultimate principle is the direct and separated object effect of microwave, and the activation of microwave causes the response difference of heterogeneity in the sample matrices to make extract and matrix sharp separation, and reaches higher yields.Microwave-assisted extract have the time short, efficient is high, widely applicable, solvent load is few etc., and advantage, particularly microwave-assisted are extracted low and easy the realizations industry amplification of facility investment, this is particularly important for the material that will carry out mass disposal.Aspect the Biological resources development and use, microwave auxiliary extraction technology has been used to extract bioactive ingredients such as vegetable phenol, flavones and polysaccharide.But utilize microwave auxiliary extraction technology chlorogenic acid extracting from sunflower seed dregs to yet there are no report.
Summary of the invention:
The objective of the invention is deficiencies such as long for the extraction time that overcomes above-mentioned prior art, that the extraction yield is low, provide a kind of microwave auxiliary reflux extractive technique to prepare the method for chlorogenic acid.
Above-mentioned purpose of the present invention realizes by following technique means: sunflower seed dregs is crushed to certain fineness, mix with a certain amount of aqueous ethanolic solution, adopt the microwave auxiliary reflux chlorogenic acid extracting of certain power, extract the end back and be cooled to room temperature rapidly with cold water, centrifugal removal residue, the extracting solution concentrating under reduced pressure reclaims solvent, and concentrated solution lyophilize or spraying drying obtain the chlorogenic acid product.
Said sunflower seed dregs smashing fineness is the 20-100 order in the aforesaid method.
Said extraction agent aqueous ethanolic solution concentration is 30%-70% (v/v) in the aforesaid method, and the solid-liquid ratio of extraction is 1: 6 to 1: 18 (w/v).
Said microwave frequency 2450MHz in the aforesaid method, microwave extraction power be 200W to 700W, extraction time is 20-60min.
Said centrifuging in the aforesaid method, concentrated and spray drying process to extracting solution, be that extracting solution is filtered with the cloth bag type whizzer, and filtrate is concentrated in vacuo to dry substance concentration under vacuum tightness 0.05-0.095MPa, 60 ℃ be 30% (w/w), and spraying drying obtains the chlorogenic acid product again.The yield of chlorogenic acid reaches 1.83%-2.12% in the product.
The advantage that the present invention had is: the method that adopts the microwave auxiliary reflux chlorogenic acid extracting, but leaching process microwave continuous action, extraction time is short, efficient is high, solvent load is few, and the chlorogenic acid yield is 1.54 times to 2.39 times of traditional alcohol solvent extraction method in the product.
Description of drawings
Fig. 1 is the device synoptic diagram of extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux of the present invention, 1-return line condensing water inlet wherein, 2-return line condensation-water drain, 3-microwave power knob, 4-working hour knob 5-microwave radiation direction, 6-extraction flask, 7-viewing window.
Embodiment
The present invention is further elaborated below in conjunction with embodiment; but the invention is not restricted to following embodiment; for persons skilled in the art; the any conspicuous change of under the prerequisite that does not deviate from the principle of the invention it being done all belongs to the protection domain of design of the present invention and claims.
Get 100g and be crushed to 20 order sunflower seed dregs, mix with 50% (v/v) aqueous ethanolic solution of 600mL, adopt the microwave auxiliary reflux chlorogenic acid extracting 30min of microwave frequency 2450MHz, power 300W, extract the end back and be cooled to room temperature rapidly with cold water, adopt the centrifugal removal residue of cloth bag type whizzer, extracting solution 0.095MPa, 60 ℃ of following vacuum concentration are concentrated in vacuo to 30% (w/w) and reclaim solvent, and the concentrated solution spraying drying obtains the chlorogenic acid product.Measure chlorogenic acid content in the product, calculate the chlorogenic acid yield.The measuring method of chlorogenic acid is in the product: adopt the ultraviolet-visible pectrophotometer method, under wavelength 325nm, measure its absorbancy with chlorogenic acid mark product earlier and obtain regression equation, again sample is dissolved in ethanolic soln and measures absorbancy, substitution regression equation calculation chlorogenic acid content, chlorogenic acid contents are the per-cent that the chlorogenic acid quality accounts for raw material sunflower seed dregs quality in the product.
Simultaneously do not apply microwave, adopt 50% (v/v) aqueous ethanolic solution lixiviate chlorogenic acid, carry out controlled trial, and measure the yield of chlorogenic acid in the product according to above-mentioned processing condition.
Two kinds of methods prepare the chlorogenic acid of sunflower seed dregs result and contrast as shown in table 1.
Table 1 applies microwave and does not add the comparison of microwave extraction chlorogenic acid of sunflower seed dregs
| The microwave auxiliary reflux method | Solvent extraction method | |
| Chlorogenic acid yield (%) | ??1.83 | ??0.91 |
By the result as seen, under identical condition, the chlorogenic acid of microwave auxiliary reflux extraction method extraction yield is 2.03 times of solvent extraction method.
Get 75g and be crushed to 40 purpose sunflower seed dregs, mix with 30% (v/v) aqueous ethanolic solution of 600mL, adopt the microwave auxiliary reflux chlorogenic acid extracting 20min of microwave frequency 2450MHz, power 500W, extract the end back and be cooled to room temperature rapidly with cold water, adopt the centrifugal removal residue of cloth bag type whizzer, be concentrated in vacuo to 30% (w/w) under the extracting solution 0.05MPa, 60 ℃ and reclaim solvent, the concentrated solution spraying drying obtains the chlorogenic acid product.Measure chlorogenic acid content in the product, calculate the chlorogenic acid yield.Simultaneously do not apply microwave solvent lixiviate chlorogenic acid, carry out controlled trial, and measure the yield of chlorogenic acid in the product according to above-mentioned processing condition.
Two kinds of methods prepare the chlorogenic acid of sunflower seed dregs result and contrast as shown in table 2.
Table 2 applies microwave and does not add the comparison of microwave extraction chlorogenic acid of sunflower seed dregs
| The microwave auxiliary reflux method | Solvent extraction method | |
| Chlorogenic acid yield (%) | ??1.94 | ??1.04 |
By the result as seen, under identical condition, the chlorogenic acid of microwave auxiliary reflux extraction method extraction yield is 1.86 times of solvent extraction method.
Get 50g and be crushed to 60 purpose sunflower seed dregs, mix with 70% (v/v) aqueous ethanolic solution of 600mL, adopt the microwave auxiliary reflux chlorogenic acid extracting 60min of microwave frequency 2450MHz, power 200W, extract the end back and be cooled to room temperature rapidly with cold water, adopt the centrifugal removal residue of cloth bag type whizzer, be concentrated in vacuo to 30% (w/w) under the extracting solution 0.08MPa, 60 ℃ and reclaim solvent, the concentrated solution lyophilize obtains the chlorogenic acid product.Measure chlorogenic acid content in the product, calculate the chlorogenic acid yield.Simultaneously do not apply microwave solvent lixiviate chlorogenic acid, carry out controlled trial, and measure the yield of chlorogenic acid in the product according to above-mentioned processing condition.
Two kinds of methods prepare the chlorogenic acid of sunflower seed dregs result and contrast as shown in table 3.
Table 3 applies microwave and does not add the comparison of microwave extraction chlorogenic acid of sunflower seed dregs
| The microwave auxiliary reflux method | Solvent extraction method | |
| Chlorogenic acid yield (%) | ??1.89 | ??1.22 |
By the result as seen, under identical condition, the chlorogenic acid of microwave auxiliary reflux extraction method extraction yield is 1.54 times of solvent extraction method.
Get 40g and be crushed to 40 purpose sunflower seed dregs, mix with 60% (v/v) aqueous ethanolic solution of 600mL, adopt the microwave auxiliary reflux chlorogenic acid extracting 20min of microwave frequency 2450MHz, power 700W, extract the end back and be cooled to room temperature rapidly with cold water, adopt the centrifugal removal residue of cloth bag type whizzer, be concentrated in vacuo to 30% (w/w) under the extracting solution 0.095MPa, 60 ℃ and reclaim solvent, the concentrated solution lyophilize obtains the chlorogenic acid product.Measure chlorogenic acid content in the product, calculate the chlorogenic acid yield.Simultaneously do not apply microwave solvent lixiviate chlorogenic acid, carry out controlled trial, and measure the yield of chlorogenic acid in the product according to above-mentioned processing condition.
Two kinds of methods prepare the chlorogenic acid of sunflower seed dregs result and contrast as shown in table 4.
Table 4 applies microwave and does not add the comparison of microwave extraction chlorogenic acid of sunflower seed dregs
| The microwave auxiliary reflux method | Solvent extraction method | |
| Chlorogenic acid yield (%) | ??2.08 | ??0.87 |
By the result as seen, under identical condition, the chlorogenic acid of microwave auxiliary reflux extraction method extraction yield is 2.39 times of solvent extraction method.
Get 33.3g and be crushed to 100 purpose sunflower seed dregs, mix with 40% (v/v) aqueous ethanolic solution of 600mL, adopt the microwave auxiliary reflux chlorogenic acid extracting 40min of microwave frequency 2450MHz, power 350W, extract the end back and be cooled to room temperature rapidly with cold water, adopt the centrifugal removal residue of cloth bag type whizzer, extracting solution concentrating under reduced pressure to 30% (w/w) reclaims solvent, and the concentrated solution lyophilize obtains the chlorogenic acid product.Measure chlorogenic acid content in the product, calculate the chlorogenic acid yield.Simultaneously do not apply microwave solvent lixiviate chlorogenic acid, carry out controlled trial, and measure the yield of chlorogenic acid in the product according to above-mentioned processing condition.
Two kinds of methods prepare the chlorogenic acid of sunflower seed dregs result and contrast as shown in table 5.
Table 5 applies microwave and does not add the comparison of microwave extraction chlorogenic acid of sunflower seed dregs
| The microwave auxiliary reflux method | Solvent extraction method | |
| Chlorogenic acid yield (%) | ??2.12 | ??1.13 |
By the result as seen, under identical condition, the chlorogenic acid of microwave auxiliary reflux extraction method extraction yield is 1.88 times of solvent extraction method.
Claims (3)
1. the method for an extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux, it is characterized in that carrying out: sunflower seed dregs is crushed to the 20-100 order according to following step, mix with a certain amount of aqueous ethanolic solution, adopt the microwave auxiliary reflux chlorogenic acid extracting of certain power, after extracting end extracting solution is filtered with the cloth bag type whizzer, and filtrate is concentrated in vacuo to dry substance concentration under 0.05-0.095MPa vacuum tightness, 60 ℃ be 30% in mass, and spraying drying obtains the chlorogenic acid product again.
2. the method for a kind of extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux according to claim 1, it is characterized in that: extraction agent aqueous ethanolic solution concentration is that by volume is 30%-70%, extracts solid-liquid ratio for to count 1 with quality and volume ratio: 6-1: 18.
3. the method for a kind of extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux according to claim 1 is characterized in that: microwave frequency 2450MHz, microwave extraction power be 200W to 700W, extraction time is 20-60min.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910184594A CN101638366A (en) | 2009-08-31 | 2009-08-31 | Method for extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910184594A CN101638366A (en) | 2009-08-31 | 2009-08-31 | Method for extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN101638366A true CN101638366A (en) | 2010-02-03 |
Family
ID=41613572
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN200910184594A Pending CN101638366A (en) | 2009-08-31 | 2009-08-31 | Method for extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101638366A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102578452A (en) * | 2012-02-20 | 2012-07-18 | 北京绿源求证科技发展有限责任公司 | Skin-nourishing nutritional food |
| CN105384632A (en) * | 2015-10-19 | 2016-03-09 | 新疆大学 | Preparation method for sunflower seed meal chlorogenic acid and applications thereof |
| CN106349074A (en) * | 2016-08-30 | 2017-01-25 | 宁夏沃福百瑞枸杞产业股份有限公司 | Method for extracting chlorogenic acid in Chinese wolfberry via microwave-assisted ultrasonic |
-
2009
- 2009-08-31 CN CN200910184594A patent/CN101638366A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102578452A (en) * | 2012-02-20 | 2012-07-18 | 北京绿源求证科技发展有限责任公司 | Skin-nourishing nutritional food |
| CN102578452B (en) * | 2012-02-20 | 2013-05-01 | 北京绿源求证科技发展有限责任公司 | Skin-nourishing nutritional food |
| CN105384632A (en) * | 2015-10-19 | 2016-03-09 | 新疆大学 | Preparation method for sunflower seed meal chlorogenic acid and applications thereof |
| CN105384632B (en) * | 2015-10-19 | 2017-06-16 | 新疆大学 | A kind of preparation method and applications of chlorogenic acid of sunflower seed dregs |
| CN106349074A (en) * | 2016-08-30 | 2017-01-25 | 宁夏沃福百瑞枸杞产业股份有限公司 | Method for extracting chlorogenic acid in Chinese wolfberry via microwave-assisted ultrasonic |
| CN106349074B (en) * | 2016-08-30 | 2019-09-24 | 宁夏沃福百瑞枸杞产业股份有限公司 | The method of microwave-assisted ultrasonic extraction fructus lycii Content of Chlorogenic Acid |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN105176137B (en) | A kind of method for separating and preparing of cape jasmine oily, water-soluble gardenin and Gardenoside | |
| CN101113147B (en) | Method for tea by-product resource utilization | |
| CN102924240B (en) | Method for extracting total magnolol according to alcoholic-alkaline method | |
| CN102827299B (en) | Efficient extraction and purification method for kumquat polysaccharide | |
| CN101838343A (en) | Method for preparing pectin by using waste sisal dregs | |
| CN102276679A (en) | Method for extracting high-purity tea saponin from oil-tea-cake by decompression boiling | |
| CN102351961A (en) | Method for extracting rhizoma polygonati polysaccharide from stems and leaves of rhizoma polygonati | |
| CN101265161A (en) | Technique for extracting cynamorlum herba cistanches medicinal materials effective component | |
| WO2020073975A1 (en) | Method for extracting marigold flavonoid in industrialized manner and marigold flavonoid thereof | |
| CN102492054B (en) | Preparation method of soybean episperm pectin gel polysaccharide | |
| CN101829501A (en) | Combined membrane filtering method for Chinese traditional medicine extraction, separation and concentration | |
| CN101982471B (en) | Technological process for extracting aucubin from fruits of eucommia ulmoides oliver | |
| CN101638366A (en) | Method for extracting chlorogenic acid of sunflower seed dregs by microwave auxiliary reflux | |
| CN109966327A (en) | A kind of method of the double assisted extraction passionflower seed oil meal general flavones of ultrasonic wave, microwave | |
| CN101955479A (en) | Method for extracting orientin from bamboo leaf | |
| CN103980730A (en) | Preparation method for high-purity pitaya pigment | |
| CN105418782A (en) | Microwave-assisted extraction technology of polygonatum sibiricum polysaccharides | |
| CN103463160A (en) | Preparation method of high-content total flavones of chrysanthemum | |
| CN102988465A (en) | Process for low-temperature extracting kudzu root flavanone and kudzu root starch from kudzu root | |
| CN101057905A (en) | Microwave extraction method for cordate houttuynia total flavones | |
| CN104926719A (en) | Method for extracting gynesine from fructus cannabis | |
| CN102327325A (en) | Method for preparing white mulberry rootbark general flavone | |
| CN101433322B (en) | Functional food rich in anthocyanidin and preparation method thereof | |
| CN100482196C (en) | An extraction preparation method of effective ingredients of Chinese medicine | |
| CN105566944A (en) | Method for separating decolorized chilli extract and chili pigments from chilli extract crude product |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20100203 |