CN104558072A - Method for extracting hesperidin in dried tangerine or orange peel by using enzymolysis approach - Google Patents
Method for extracting hesperidin in dried tangerine or orange peel by using enzymolysis approach Download PDFInfo
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- CN104558072A CN104558072A CN201410624367.0A CN201410624367A CN104558072A CN 104558072 A CN104558072 A CN 104558072A CN 201410624367 A CN201410624367 A CN 201410624367A CN 104558072 A CN104558072 A CN 104558072A
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- hesperidin
- orange peel
- enzymolysis
- pectin
- dried tangerine
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Abstract
The invention provides a method for extracting hesperidin in dried tangerine or orange peel by using an enzymolysis approach and relates to the field of medicines. Because citrus and other peels are enriched in pectin, and dissolution of active ingredients in cells is hindered by the pectin. According to the method disclosed by the invention, the pectin between cell walls of medicinal materials and cells is subjected to enzymolysis by adopting pectinase, so that the cell wells are destroyed, the hesperidin is fully dissolved, and the aim of obviously improving the hesperidin extraction rate is achieved. The method can be used for extracting the hesperidin in medicinal materials such as the dried tangerine or orange peel, fructus aurantii and immature bitter orange. The method disclosed by the invention has the advantages that the operation is simple, organic solvent residues are avoided, the environmental pollution is avoided, special equipment is not needed, the production safety is high, large-scale enterprise production is promoted, and the like.
Description
Technical field
The invention provides a kind of method that enzymolysis process extracts Hesperidin, relate to field of medicaments.
Background technology
Hesperidin has reduction vascular fragility, hypotensive, the effect such as antianaphylaxis, Tumor suppression, clinically for the assisting therapy of cardiovascular system diseases, also can be used for the raw material of pharmacy in medicine industry, Hesperidin is also used for foods and cosmetics industry as natural antioxidants.
Tradition extracts from peel of Citrus reticulata Blanco that Hesperidin adopts that hot water extraction, alcohol reflux extract usually, alkali puies forward the methods such as acid is heavy.These methods are all adopt chemical solvents to infiltrate the effective constituent of dissolving in medicinal material, although simple to operation, existence is extracted not exclusively, caused some Hesperidins to remain in pomace, and the chemical reagent of use easily causes the shortcomings such as environmental pollution.Report microwave and ultrasound assisted extraction Hesperidin in recent years.Although these two kinds of method extraction times are short, ultrasonic method noise is very large, and microwave method has radiation, and they have very high requirement to extraction equipment, and this limits its application in the large production of enterprise to a certain extent.
About containing 30% pectin in the pericarps such as oranges and tangerines, lemon, shaddock, pectin is mainly present in cell walls and the cell internal layer of plant, because pectin hinders the stripping of the effective constituent such as Hesperidin in cell, adopt polygalacturonase can enzymolysis pectin, Hesperidin is dissolved out fully, thus significantly improves the extraction yield of Hesperidin.
With traditional method as compared with alcoholic solvent reflux extraction, enzymolysis process extracts Hesperidin and has easy filtration, and simple to operate, organic solvent-free remains, and does not cause the advantage of environmental pollution.Compared with ultrasonic extraction, microwave loss mechanisms, that it has is good without the need to specific installation, production security, be conducive to labour protection and be conducive to the advantages such as the large production of enterprise.
Summary of the invention
A kind of enzymolysis process extracts the method for Hesperidin in dried orange peel, it is characterized in that: take dried orange peel medicinal material coarse powder appropriate, the ratio being 1: 8 ~ 40 (g/mL) according to solid-liquid ratio adds distilled water, be that 0 ~ 3% of quality of medicinal material adds polygalacturonase according to consumption, its consumption is 0 ~ 3% of quality of medicinal material, with dilute hydrochloric acid, the pH value of liquid is adjusted to 3 ~ 5, be placed in 40 ~ 55 DEG C of waters bath with thermostatic control 0 ~ 3 hour, take out, filter, filtrate is concentrated into medicinal extract, is then placed in vacuum drying oven and is dried to powder, obtains Hesperidin extract.
Embodiment
Below in conjunction with embodiment, the present invention is further described, but it is not represented as unique embodiment of the present invention.
Embodiment one
1. the extraction of Hesperidin:
Dried orange peel medicinal material is shattered into meal, take 100.00g, add 300mL distilled water, add polygalacturonase (300000U/g), consumption is 0.3% of quality of medicinal material, be 3 by the pH value of dilute hydrochloric acid regulator solution, be placed in 45 DEG C of constant water bath box enzymolysis 2 hours, take out, filter, filtrate is concentrated into medicinal extract, is then placed in vacuum and is dried to powder in dry case, obtain Hesperidin extract.
2. the assay of Hesperidin in extract
Adopt HPLC method to measure, measuring method records method with reference to the content of Hesperidin in version " Chinese Pharmacopoeia " dried orange peel medicinal material in 2010.
(1) preparation of standardized solution accurately takes Hesperidin standard substance 10.1mg, adds proper amount of methanol, ultrasonic dissolution, by methanol constant volume to 25mL, is mixed with the Hesperidin standard solution that mass concentration is 0.404mg/mL.
(2) determination of determined wavelength is with blank solvent methyl alcohol for reference solution, is scanned Hesperidin standardized solution by ultraviolet-visible pectrophotometer between 200 ~ 400nm wavelength, meanwhile, also carries out spectral scan to dried orange peel sample solution.Result shows, and Hesperidin standardized solution and dried orange peel sample liquid all have strong absorption peak at 285nm place, and therefore getting 283nm is determined wavelength.
(3) HPLC chromatographic condition chromatographic column: Waters Symmetry C18 (250mm × 4.6mm, 5 μm), moving phase: methyl alcohol-2% glacial acetic acid solution (34: 66), flow velocity: 0.5mL/min, determined wavelength: 283nm, temperature is room temperature.Sample size: 20 μ L.Hesperidin retention time is 5.1min.
(4) preparation of typical curve
Respectively accurate draw Hesperidin standardized solution 1,2,3,4,5mL is in the volumetric flask of 10mL, by methanol constant volume, be made into the series of standards solution that mass concentration is respectively 40.4,80.8,121.2,161.6,202 μ g/mL, carry out HPLC mensuration, survey peak area at 283nm wavelength place.With the concentration of Hesperidin standardized solution (μ g/mL) for X-coordinate, with its peak area for ordinate zou drawing standard curve, obtaining regression equation is y=185220x-25642, R
2=0.999, wherein y represents peak area, and x represents the concentration of Hesperidin.Linearity range is 40.4 ~ 202 μ g/mL.
(5) mensuration of Hesperidin extraction yield
Extract gained solution, with 0.45 μm of filtering with microporous membrane, survey its peak area by HPLC.By the content of Hesperidin in regression equation calculation sample.In triplicate, average, recording Hesperidin in Hesperidin extract has 5.58g, then the extraction yield of Hesperidin is 5.58% in experiment.
Embodiment two
1. the extraction of Hesperidin:
Take dried orange peel medicinal material medicinal material coarse powder 100g, add 200mL distilled water, add polygalacturonase (30000U/g), consumption is 3% of quality of medicinal material, is 4 by the pH value of dilute hydrochloric acid regulator solution, be placed in 45 DEG C of constant water bath box enzymolysis 1.5 hours, take out, filter, filtrate is concentrated into medicinal extract, then be placed in vacuum drying oven and be dried to powder, obtain Hesperidin extract.
2. the mensuration of Hesperidin extraction yield
Measure according to above HPLC method, recording Hesperidin in Hesperidin extract has 5.02g, then the extraction yield of Hesperidin is 5.02%.
Claims (1)
1. the method for Hesperidin in an enzymolysis and extraction dried orange peel, it is characterized in that: take dried orange peel medicinal material coarse powder appropriate, the ratio being 1: 8 ~ 40 (g/mL) according to solid-liquid ratio adds distilled water, is that 0 ~ 3% of quality of medicinal material adds polygalacturonase, with dilute hydrochloric acid, the pH value of liquid is adjusted to 3 ~ 5 according to consumption, be placed in 40 ~ 55 DEG C of water bath with thermostatic control enzymolysis 0 ~ 3 hour, take out, filter, filtrate is concentrated into medicinal extract, then be placed in vacuum drying oven and be dried to powder, obtain Hesperidin extract.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201410624367.0A CN104558072A (en) | 2014-10-31 | 2014-10-31 | Method for extracting hesperidin in dried tangerine or orange peel by using enzymolysis approach |
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| CN201410624367.0A CN104558072A (en) | 2014-10-31 | 2014-10-31 | Method for extracting hesperidin in dried tangerine or orange peel by using enzymolysis approach |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105053952A (en) * | 2015-08-31 | 2015-11-18 | 大闽食品（漳州）有限公司 | Processing technology of dried tangerine peel extract without bitter taste |
| CN113072599A (en) * | 2021-03-10 | 2021-07-06 | 武汉市华甜生物科技有限公司 | Method for preparing natural hesperidin by biological fermentation and extraction |
| CN113651791A (en) * | 2021-09-01 | 2021-11-16 | 湖南华诚生物资源股份有限公司 | Method for separating hesperetin from immature bitter orange |
| CN114451537A (en) * | 2022-02-22 | 2022-05-10 | 广东橘香斋大健康产业股份有限公司 | Preparation process of dried orange peel and autumn pear paste |
| WO2022165994A1 (en) * | 2021-02-08 | 2022-08-11 | 华南农业大学 | Pericarpium citri reticulatae chachiensis extract, preparation method therefor and use thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467547A (en) * | 2013-09-17 | 2013-12-25 | 南京通泽农业科技有限公司 | Novel method for extracting hesperidin from orange peel |
| CN103483404A (en) * | 2013-09-24 | 2014-01-01 | 重庆主流生物工程有限公司 | Method for extracting and purifying hesperidin from orange residues |
-
2014
- 2014-10-31 CN CN201410624367.0A patent/CN104558072A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103467547A (en) * | 2013-09-17 | 2013-12-25 | 南京通泽农业科技有限公司 | Novel method for extracting hesperidin from orange peel |
| CN103483404A (en) * | 2013-09-24 | 2014-01-01 | 重庆主流生物工程有限公司 | Method for extracting and purifying hesperidin from orange residues |
Non-Patent Citations (1)
| Title |
|---|
| NOBUYA INABA ET AL.: "Extraction and Recovery of Hesperidin from Peel Residue of Satsuma Mandarin(Citrus unshiu marc.) Using Enzymes", 《NIPPON SHOKUHIN KOGYO GAKKAISHI》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105053952A (en) * | 2015-08-31 | 2015-11-18 | 大闽食品（漳州）有限公司 | Processing technology of dried tangerine peel extract without bitter taste |
| CN105053952B (en) * | 2015-08-31 | 2017-12-19 | 大闽食品（漳州）有限公司 | A kind of processing technology of the dried orange peel extracts of no bitter taste |
| WO2022165994A1 (en) * | 2021-02-08 | 2022-08-11 | 华南农业大学 | Pericarpium citri reticulatae chachiensis extract, preparation method therefor and use thereof |
| CN113072599A (en) * | 2021-03-10 | 2021-07-06 | 武汉市华甜生物科技有限公司 | Method for preparing natural hesperidin by biological fermentation and extraction |
| CN113651791A (en) * | 2021-09-01 | 2021-11-16 | 湖南华诚生物资源股份有限公司 | Method for separating hesperetin from immature bitter orange |
| CN114451537A (en) * | 2022-02-22 | 2022-05-10 | 广东橘香斋大健康产业股份有限公司 | Preparation process of dried orange peel and autumn pear paste |
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Application publication date: 20150429 |