CN102492007A - Method for extracting flavones compounds and total phenol from hot pepper residue - Google Patents
Method for extracting flavones compounds and total phenol from hot pepper residue Download PDFInfo
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- CN102492007A CN102492007A CN2011104062910A CN201110406291A CN102492007A CN 102492007 A CN102492007 A CN 102492007A CN 2011104062910 A CN2011104062910 A CN 2011104062910A CN 201110406291 A CN201110406291 A CN 201110406291A CN 102492007 A CN102492007 A CN 102492007A
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Abstract
The invention discloses a method for extracting flavones compounds and total phenol from hot pepper residue. The method comprises the following steps of: extracting the hot pepper residue by using an aqueous solution of ethanol to obtain leaching liquor; centrifuging the leaching liquor to obtain supernatant; microfiltering the supernatant to obtain a filtrate; and concentrating the filtrate until the filtrate is dry to obtain a product. The invention has the advantages that: the method is low is cost, economic and the like, the source of raw materials is wide, the process is simple and feasible, and extracting conditions are reasonable; the production and using processes meet the requirements of the national safe food production; and the method has a good industrialization prospect, and higher implementation value as well as social and economic benefits.
Description
Technical field
The present invention relates to a kind of method of from hot chili residue, extracting flavonoid compound and total phenol.
Background technology
China's capsicum aboundresources, the overwhelming majority of manufacturing enterprise serves as theme with the production of paprika oleoresin, capsochrome etc., and its advantage is that quality better, the quality of production are stable, production is easy to control, but significant disadvantages is also arranged, and promptly product yield is low, quality is low, and waste is serious.
Contain rich nutrient substances in the pepper fruit.According to surveying and determination, the main nutrient composition in the capsicum has vitamins C, vitamin A, vitamin G, soluble sugar, protein, Serlabo, nicotinic acid etc., also contains mineral elements such as abundant calcium, phosphorus, iron.The composition of the antioxidant in the capsicum is cinnamic acid derivatives such as flavonoid and coffic acid, chlorogenicacid; Containing abundant antioxidant vitamins in the capsicum pericarp in addition, mainly contain vitamin E (Viteolin), vitamins C (xitix) and β-Hu Luobusu (vitamin a source), is the high-quality natural antioxidants of generally acknowledging, the polyphenoils in the capsicum belongs to phenol type material.
Effects such as that polyphenolic compound has is anti-oxidant, antibiotic, antitumor, anticancer, reducing blood-fat, hypoglycemic and prevention cardiovascular and cerebrovascular diseases; Caused the interest of increasing researcher, in industry extensive application such as food, healthcare products, makeup and medicine.
Hot chili residue is the by product of capsicum pericarp processing, wherein contains rich nutrient contents, and annual China all has a large amount of hot chili residues to be abandoned as industrial waste, or uses as feed.Not only environment is exerted a certain influence, and cause the very big wasting of resources.Therefore, extract biologically active substance such as flavones and total phenol in the hot chili residue, help the comprehensive utilization of capsicum resource, can improve the added value of capsicum.
Summary of the invention
The purpose of this invention is to provide a kind of method of from hot chili residue, extracting flavonoid compound and total phenol.
A kind of method of from hot chili residue, extracting flavonoid compound and total phenol provided by the invention, comprise the steps: with aqueous ethanolic solution to said hot chili residue extract vat liquor; Said vat liquor is carried out the centrifugal supernatant that gets; Said supernatant is carried out micro-filtration must filtrate; Concentrate said filtrating and promptly get product to doing.
In the above-mentioned method, the granularity of said hot chili residue can be 20 orders～80 orders, specifically can be 20 orders, 30 orders or 60 orders.
In the above-mentioned method, alcoholic acid quality percentage composition can be 10%～90% in the said aqueous ethanolic solution, specifically can be 40%, 50% or 90%.
In the above-mentioned method, the ratio of quality and the number of copies of said aqueous ethanolic solution and said hot chili residue can be (5～20): 1, specifically can be 5: 1,10: 1 or 20: 1.
In the above-mentioned method, the temperature of said extraction can be 20 ℃～80 ℃, specifically can be 30 ℃, 40 ℃ or 60 ℃; The time of said extraction can be 1 hour～and 7 hours, specifically can be 4 hours or 6 hours.
In the above-mentioned method, said extraction can be carried out in the water bath with thermostatic control shaking table; The oscillation frequency of said water bath with thermostatic control shaking table can be 80r/min～150r/min, specifically can be 80r/min, 100r/min or 150r/min.
In the above-mentioned method, the rotating speed of said centrifugal treating can be 3800～4200r/min, specifically can be 4000r/min or 4200r/min, and the time of said centrifugal treating can be 5min～20min, specifically can be 15min or 20min.
In the above-mentioned method, the aperture that said micro-filtration is handled with microporous membrane can be 0.22 μ m～0.45 μ m, specifically can be 0.22 μ m or 0.45 μ m.
In the above-mentioned method, said spissated temperature can be 45 ℃～80 ℃, specifically can be 50 ℃, 65 ℃ or 75 ℃.
The flavonoid compound that method provided by the invention is extracted can be rutin, and total phenol can be gallic acid.
In the method provided by the invention; Raw material sources are extensive, simple for process, extraction conditions is reasonable, expense is low, the economic dispatch advantage; Production and use all meet the requirement of national security foodstuff production, and excellent industrial application foreground is arranged, and have bigger implementary value and economic results in society.
Embodiment
Employed experimental technique is ordinary method like no specified otherwise among the following embodiment.
Used material, reagent etc. like no specified otherwise, all can obtain from commercial sources among the following embodiment.
The concrete grammar that content of flavonoids is measured among the following embodiment is: the sample 0.5mL that gets proper concn; Add in the 15mL scale test tube, be supplemented to 4mL with deionized water, the sodium nitrite in aqueous solution that adds 0.3mL 5% (w/v) shakes up; Adding 3mL 1% (w/v) aluminum chloride aqueous solution behind the 5min shakes up; Add the aqueous sodium hydroxide solution of the 1mol/L of 2mL behind the 6min, add deionized water again to 10mL, the 510nm place measures light absorption value behind the 10min; Blank replaces sample to react with deionized water; Content of flavonoids is represented with rutin equivalent (Rutin Equivalent, RE/g butt).
The preparation of standardized solution: accurately take by weighing rutin mark article 0.075g, in the volumetric flask as for 25mL, it is settled to scale with methyl alcohol.Pipette 5mL, 4mL, 3mL, 2mL and 1mL respectively in the 10mL volumetric flask with transfer pipet then; With methanol constant volume to scale; Obtain concentration and be respectively 1.5,1.2,0.9,0.6 and the solution of 0.3mg/mL; Measure according to the method described above, maximum absorption is arranged, obtain the typical curve between the concentration of absorbance and rutin mark article at 510nm place at the 510nm place.
The extract that embodiment 1～3 obtains is measured according to the method described above, can be obtained content of flavonoids in the extract according to the typical curve that obtains.
The concrete grammar of the assay of total phenol is among the following embodiment: get certain density sample 0.5mL; Add 2.5mL 0.2N Folin-Ciocalteu reagent; Vibration 20s afterreaction 5min; The aqueous sodium carbonate solution that adds 2mL 7.5% (w/v) again, vibration 20s afterreaction 2h measures absorbancy at the 760nm place; Blank replaces sample to react with deionized water; Total phenol content is represented with gallic acid equivalant (Gallic Acid Equivalent, GAE/g butt).
The preparation of standardized solution: accurately take by weighing Nutgalls acidity scale article 0.0085g in the volumetric flask of 50mL, it is settled to scale with deionized water; Pipette 5mL, 4mL, 3mL, 2mL and 1mL respectively in the 10mL volumetric flask with transfer pipet then; Be settled to scale with deionized water; Obtain concentration and be respectively 0.085,0.068,0.051,0.034 and the solution of 0.017mg/mL; Measure according to the method described above, maximum absorption is arranged, obtain the typical curve between the concentration of absorbance and Nutgalls acidity scale article at 760nm place at the 760nm place.
The extract that embodiment 1～3 obtains is measured according to the method described above, can be obtained the content of total phenol in the extract according to the typical curve that obtains.
The extraction of embodiment 1, flavonoid compound and total phenol
(1) pre-treatment: at first hot chili residue is pulverized the back and dry naturally, then siccative is crossed 60 mesh sieves;
(2) solvent extraction: take by weighing 100g and add in the Erlenmeyer flask through pretreated hot chili residue; With the aqueous ethanolic solution is to extract medium; Add 10 times to the hot chili residue quality, alcoholic acid quality percentage composition is 40% aqueous ethanolic solution; Extracting temperature is 40 ℃, and (150r/min) extracts 4h to the active substance in the hot chili residue and get vat liquor in the water bath with thermostatic control shaking table, then vat liquor centrifugal 15min under 4200r/min got supernatant;
(3) micro-filtration: the supernatant that obtains is crossed the aperture must filtrate for the 0.45um microporous membrane;
(4) concentrate: it is dried to use rotatory evaporator under 75 ℃ of conditions, the filtrating behind the micro-filtration to be concentrated into, and promptly obtains containing the extract of flavonoid compound and total phenol.
Flavonoid compound and total phenol content are respectively 6.11mgRE/g and 22.13mgGAE/g in the extract that present embodiment obtains.
The extraction of embodiment 2, flavonoid compound and total phenol
(1) pre-treatment: at first hot chili residue is pulverized dry below 100 ℃, then siccative is crossed 30 mesh sieves;
(2) solvent extraction: take by weighing 100g and add in the Erlenmeyer flask through pretreated hot chili residue; With the aqueous ethanolic solution aqueous solution serves as to extract solvent; Add 5 times to the hot chili residue quality, alcoholic acid quality percentage composition is 50% aqueous ethanolic solution; Extracting temperature is 60 ℃, and (100r/min) extracts 6h to the active substance in the hot chili residue and get vat liquor in the water bath with thermostatic control shaking table, then vat liquor centrifugal 20min under 4000r/min got supernatant;
(3) micro-filtration: the supernatant that obtains is crossed the aperture must filtrate for the 0.45um microporous membrane;
(4) concentrate: it is dried to use rotatory evaporator under 65 ℃ of conditions, the filtrating behind the micro-filtration to be concentrated into, and promptly obtains containing the extract of flavonoid compound and total phenol.
Present embodiment obtains that flavonoid compound and total phenol content are respectively 4.14mgRE/g and 19.35mgGAE/g in the extract.
The extraction of embodiment 3, flavonoid compound and total phenol
(1) pre-treatment: at first hot chili residue is dried naturally, then siccative is crossed 20 mesh sieves;
(2) solvent extraction: take by weighing 100g and add in the Erlenmeyer flask through pretreated hot chili residue; With the aqueous ethanolic solution aqueous solution serves as to extract solvent; Add 20 times to the hot chili residue quality, alcoholic acid quality percentage composition is 90% aqueous ethanolic solution; Extracting temperature is 30 ℃, and (80r/min) extracts 6h to the active substance in the hot chili residue in the water bath with thermostatic control shaking table, and vat liquor centrifugal 20min under 4200r/min gets supernatant then;
(3) micro-filtration: it is that the microporous membrane of 0.22um must be filtrated that the supernatant that obtains is crossed the aperture;
(4) concentrate: it is dried to use rotatory evaporator under 50 ℃ of conditions, the filtrating behind the micro-filtration to be concentrated into, and promptly obtains containing the extract of flavonoid compound and total phenol.
Present embodiment obtains that flavonoid compound and total phenol content are respectively 3.29mgRE/g and 12.66mgGAE/g in the extract.
Claims (9)
1. a method of from hot chili residue, extracting flavonoid compound and total phenol comprises the steps:
With aqueous ethanolic solution to said hot chili residue extract vat liquor; Said vat liquor is carried out the centrifugal supernatant that gets; Said supernatant is carried out micro-filtration must filtrate; Concentrate said filtrating and promptly get product to doing.
2. method according to claim 1 is characterized in that: the granularity of said hot chili residue is 20 orders～80 orders.
3. method according to claim 1 and 2 is characterized in that: alcoholic acid quality percentage composition is 10%～90% in the said aqueous ethanolic solution.
4. according to arbitrary described method among the claim 1-3, it is characterized in that: the ratio of quality and the number of copies of said aqueous ethanolic solution and said hot chili residue is (5～20): 1.
5. according to arbitrary described method among the claim 1-4, it is characterized in that: the temperature of said extraction is 20 ℃～80 ℃; The time of said extraction is 1 hour～7 hours.
6. according to arbitrary described method among the claim 1-5, it is characterized in that: said being extracted in the water bath with thermostatic control shaking table carried out; The oscillation frequency of said water bath with thermostatic control shaking table is 80r/min～150r/min.
7. according to arbitrary described method among the claim 1-6, it is characterized in that: the rotating speed of said centrifugal treating is 3800r/min～4200r/min, and the time of said centrifugal treating is 5min～20min.
8. according to arbitrary described method among the claim 1-7, it is characterized in that: said micro-filtration is handled and used the aperture of microporous membrane is 0.22 μ m～0.45 μ m.
9. according to arbitrary described method among the claim 1-8, it is characterized in that: said spissated temperature is 45 ℃～80 ℃.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103926212A (en) * | 2013-01-16 | 2014-07-16 | 九芝堂股份有限公司 | Determination method for content of total phenols in callicarpa nudiflora |
| CN110759879A (en) * | 2019-11-20 | 2020-02-07 | 贵州红星山海生物科技有限责任公司 | Method for extracting natural vitamin C from chili particles |
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| CN101696381A (en) * | 2009-10-23 | 2010-04-21 | 中国科学院西北高原生物研究所 | Novel process for preparing highland barley flavone extract and application thereof in health wine |
| CN102166261A (en) * | 2011-04-13 | 2011-08-31 | 沈阳药科大学 | Clove leaf extract and method for preparing same |
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| US20020055471A1 (en) * | 2000-08-31 | 2002-05-09 | Bailey David T. | Efficient method for producing compositions enriched in anthocyanins |
| CN101696381A (en) * | 2009-10-23 | 2010-04-21 | 中国科学院西北高原生物研究所 | Novel process for preparing highland barley flavone extract and application thereof in health wine |
| CN102166261A (en) * | 2011-04-13 | 2011-08-31 | 沈阳药科大学 | Clove leaf extract and method for preparing same |
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| 张云，等: "黄珠子草不同部位总黄酮和总酚含量及抑菌活性测定", 《西北农业学报》 * |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103926212A (en) * | 2013-01-16 | 2014-07-16 | 九芝堂股份有限公司 | Determination method for content of total phenols in callicarpa nudiflora |
| CN110759879A (en) * | 2019-11-20 | 2020-02-07 | 贵州红星山海生物科技有限责任公司 | Method for extracting natural vitamin C from chili particles |
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Application publication date: 20120613 |