CN102727609A - Pear polyphenols extraction method - Google Patents
Pear polyphenols extraction method Download PDFInfo
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- CN102727609A CN102727609A CN2012102292170A CN201210229217A CN102727609A CN 102727609 A CN102727609 A CN 102727609A CN 2012102292170 A CN2012102292170 A CN 2012102292170A CN 201210229217 A CN201210229217 A CN 201210229217A CN 102727609 A CN102727609 A CN 102727609A
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Abstract
The invention relates to a pear polyphenols extraction method, falling into the field of extraction and processing of plant active substances. The method comprises the steps of peeling and stoning young pear fruits, dicing into pieces smaller than 1 cubic centimeter, grinding into powder with liquid nitrogen, soaking with 30-90% ethanol solution at sample/solution mass volume ratio of 1:(20-30), extracting on a constant temperature shaking bed in dark at 50-70 DEG C and uniform speed of 100-170 rpm for 2-6 h, and centrifuging to collect supernatant as pear polyphenols extractive solution. The extraction method adopts liquid nitrogen grinding to enable extraction process under low temperature state, to avoid oxidation reaction of pear polyphenols during grinding process and improve polyphenols activity. Through extraction with the constant temperature shaking bed under uniform speed, sufficient contact between sample and extraction solvent is facilitated to improve extraction rate by 5-17% compared with constant temperature water bath extraction.
Description
Technical field
The present invention relates to active substance of plant extraction, manufacture field, relate to a kind of pears polyphenol extracting method, be specifically related to a kind of method of utilizing solvent method from the pears young fruit, to extract plant polyphenol.
Background technology
Plant polyphenol is extensively to be present in the intravital important secondary metabolite of plant, has different physiological roles (2007) such as antioxidation, antitumor, the liver protecting.Plant polyphenol content in grain, vegetable is less, but in fruit and corn cortex content higher (2000).Pears are the third-largest fruit of China, and area and output are only second to Fructus Mali pumilae and Citrus.Because it is multiple like polyphenols (2004,2011) such as arbutin, chlorogenic acid, vanillin that it contains, therefore has certain anti-oxidation health function.Though research shows that the relative concentration that these polyphenol substances exist in ripe pear fruit is not very high, the pears young fruit contains very abundant polyphenols (2004,2009).Aborning; Because the needs of cultivation managements such as physiological fallen fruit or flower and fruit thinning; A large amount of pears young fruit abandoneds; Caused the waste of Polyphenols living resources to a certain extent, and how efficiently key how to recycle these living resources is these polyphenols of extraction and analysis, but report is not also arranged about the research of polyphenols highly effective extraction method in the pears young fruit.
Summary of the invention
The object of the present invention is to provide a kind of is raw material with the pears young fruit, obtains the extraction process of pears polyphenol through solvent method.
The object of the invention can be realized through following technical scheme:
A kind of pears polyphenol extracting method, pears young fruit peeling enucleation is cut into less than 1cm
3Fritter, use the liquid nitrogen grinding powdered; Alcoholic solution with 30% ~ 90% carries out lixiviate to melonidum; The mass volume ratio of lixiviate sample and solution is 1:20 ~ 30; With constant temperature shaking table lucifuge, 50 ℃ ~ 70 ℃, at the uniform velocity lixiviate of 100 ~ 170rpm; Each extraction time is 2 ~ 6 hours, goes out supernatant with the centrifuge centrifugalize and is pears polyphenol extracting solution.
Described pears polyphenol extracting method preferably uses 40% ~ 60% alcoholic solution that melonidum is carried out lixiviate.
Described pears polyphenol extracting method, the oscillation rate of constant temperature shaking table is preferably 100 ~ 150rpm.
Described pears polyphenol extracting method, preferred 2 ~ 4 hours of described extraction time.
Described pears polyphenol extracting method, pears young fruit refer to behind the fallen flowers 1 ~ 2 month pear fruit.
According to polyphenol content in the pears polyphenol extracting solution of the inventive method acquisition is 75mg/100g ~ 147mg/100g.
In addition; Utilize HPLC that the polyphenol substance that the present invention obtains is identified; Make standard substance with 11 kinds of chromatographically pure reference substances such as arbutin, gallic acid, catechin, chlorogenic acid, epicatechin, caffeic acid, vanillin, ferulic acid, rutin, phlorhizin, Quercetins; Do eluant with methanol and water mixed solvent,, thereby estimate the quality of extracting polyphenol according to effective ingredient in the peak area qualitative and quantitative analysis extract.It is as shown in Figure 1 that the chromatograph of standard substance goes out the peak collection of illustrative plates, and the appearance time of arbutin is about 6.8 minutes, and the appearance time of gallic acid is about 7.3 minutes; The appearance time of catechin is about 9.6 minutes, and the appearance time of chlorogenic acid is about 10.1 minutes, and the appearance time of epicatechin is about 11.0 minutes; Caffeinic appearance time is about 11.5 minutes, and the appearance time of vanillin is about 12.7 minutes, and the appearance time of ferulic acid is about 13.5 minutes; The rutin appearance time is about 14.4 minutes; The phlorhizin appearance time is about 15.4 minutes, and the Quercetin appearance time is about 21.8 minutes, and the chromatograph of sample goes out the peak collection of illustrative plates and sees Fig. 2.
Beneficial effect of the present invention:
1, adopt the liquid nitrogen grinding sample, can make sample mill get more carefully, more abundant, extraction ratio is increased.
2, liquid nitrogen grinding makes leaching process be in low temperature state, has avoided the pears polyphenol that oxidation reaction takes place in process of lapping, improves the activity of polyphenol.
3, leaching process uses the at the uniform velocity lixiviate of constant temperature shaking table, is beneficial to sample and fully contacts with the extraction solvent, and extraction ratio improves 5%-17% than water bath with thermostatic control.
Description of drawings
Fig. 1 goes out the peak collection of illustrative plates for the chromatograph of standard substance
1 is arbutin, and appearance time is about 6.8 minutes; 2 is gallic acid, and appearance time is about 7.3 minutes; 3 is catechin, and appearance time is about 9.6 minutes; 4 is chlorogenic acid, and appearance time is about 10.1 minutes; 5 is epicatechin, and appearance time is about 11.0 minutes; 6 is caffeic acid, and appearance time is about 11.5 minutes; 7 is vanillin, and appearance time is about 12.7 minutes; 8 is ferulic acid, and appearance time is about 13.5 minutes; 9 is rutin, and appearance time is about 14.4 minutes; 10 is phlorhizin, and appearance time is about 15.4 minutes; 11 is Quercetin, and appearance time is about 21.8 minutes.
Fig. 2 goes out the peak collection of illustrative plates for the chromatograph of sample
1 is arbutin, and 2 is gallic acid, and 3 is catechin, and 4 is chlorogenic acid, and 5 is epicatechin, and 6 is caffeic acid, and 7 is vanillin, and 8 is ferulic acid, and 9 is rutin.
The specific embodiment
Embodiment 1:
Choose healthy pears young fruit, peeling, enucleation is cut into less than 1cm
3Fritter is used the liquid nitrogen flash freezer grind into powder, adds 40% alcoholic solution; Sample and solution quality volume ratio are 1:20; With constant temperature shaking table 100rpm 50 ℃ of lixiviates 2 hours (lucifuge), the centrifuge centrifugalize goes out pears polyphenol extracting solution, and it is 75mg/100g that the FC method is measured polyphenol content.
Comparative Examples 1:
Other conditions only change the lixiviate of constant temperature shaking table under the uniform temp water bath with thermostatic control lixiviate with embodiment 1, and the pears polyphenol extracting solution polyphenol content that is obtained is 71mg/100g.
Embodiment 2:
Choose healthy pears young fruit, peeling, enucleation is cut into less than 1cm
3Fritter is used the liquid nitrogen flash freezer grind into powder, adds 50% alcoholic solution; Sample and solution quality volume ratio are 1:30; With constant temperature shaking table 120rpm 50 ℃ of lixiviates 3 hours (lucifuge), the centrifuge centrifugalize goes out pears polyphenol extracting solution, and it is 90mg/100g that the FC method is measured polyphenol content.
Comparative Examples 2:
Other conditions only change the lixiviate of constant temperature shaking table under the uniform temp water bath with thermostatic control lixiviate with embodiment 2, and the pears polyphenol extracting solution polyphenol content that is obtained is 77mg/100g.
Embodiment 3:
Choose healthy pears young fruit, peeling, enucleation is cut into less than 1cm
3Fritter is used the liquid nitrogen flash freezer grind into powder, adds 50% alcoholic solution; Sample and solution quality volume ratio are 1:20; With constant temperature shaking table 150rpm 60 ℃ of lixiviates 4 hours (lucifuge), the centrifuge centrifugalize goes out pears polyphenol extracting solution, and it is 104mg/100g that the FC method is measured polyphenol content.
Comparative Examples 3:
Other conditions only change the lixiviate of constant temperature shaking table under the uniform temp water bath with thermostatic control lixiviate with embodiment 3, and the pears polyphenol extracting solution polyphenol content that is obtained is 83mg/100g.
Embodiment 4:
Choose healthy pears young fruit, peeling, enucleation is cut into less than 1cm
3Fritter is used the liquid nitrogen flash freezer grind into powder, adds 60% alcoholic solution; Sample and solution quality volume ratio are 1:30; With constant temperature shaking table 130rpm 60 ℃ of lixiviates 2 hours (lucifuge), the centrifuge centrifugalize goes out pears polyphenol extracting solution, and it is 124mg/100g that the FC method is measured polyphenol content.
Comparative Examples 4:
Other conditions only change the lixiviate of constant temperature shaking table under the uniform temp water bath with thermostatic control lixiviate with embodiment 4, and the pears polyphenol extracting solution polyphenol content that is obtained is 105mg/100g.
Embodiment 5:
Choose healthy pears young fruit, peeling, enucleation is cut into less than 1cm
3Fritter is used the liquid nitrogen flash freezer grind into powder, adds 60% alcoholic solution; Sample and solution quality volume ratio are 1:30; With constant temperature shaking table 150rpm70 ℃ of lixiviate 2 hours (lucifuge), the centrifuge centrifugalize goes out pears polyphenol extracting solution, and it is 147mg/100g that the FC method is measured polyphenol content.
Comparative Examples 5:
Other conditions only change the lixiviate of constant temperature shaking table under the uniform temp water bath with thermostatic control lixiviate with embodiment 5, and the pears polyphenol extracting solution polyphenol content that is obtained is 122mg/100g.
Embodiment 6: the quantitative and qualitative analysis of pears polyphenol extract
The instrument high performance liquid chromatograph that this experiment is adopted: Waters1525.Efficient liquid phase chromatographic analysis condition: chromatographic column, C18 post 150mm * 4.6mm, Φ 5 μ m; Mobile phase, the first alcohol and water; Column temperature, 30 ℃; Flow velocity, 0.6mLmin
-1Sample size, 5 μ L; UV-detector, wavelength 280nm.Mobile phase A: water, transfer pH3.2 with phosphoric acid; B: methanol.The linear gradient leaching program, the time (min)/B (%): 0/2,3/2,4/25,11/50,16/80,26/80,30/2,35/2.Standard specimen arbutin, gallic acid, catechin, chlorogenic acid, epicatechin, caffeic acid, vanillin, ferulic acid, rutin, phlorhizin, 11 kinds of standard substance of Quercetin are chromatographically pure available from Sigma company.
The standard substance preparation: accurately take by weighing standard substance, be configured to 0.005mg/ml, 0.025mg/ml, 0.0625mg/ml, 0.125mg/ml, 0.25mg/ml, 0.5mg/ml Concentraton gradient with 50% methanol solution, cross 0.45 μ m filter membrane, the machine of treating is used.
Sample preparation: get the extracting solution 30ml that centrifugalize goes out among the embodiment 5 and use the Rotary Evaporators evaporate to dryness, to 2ml, cross 0.45 μ m filter membrane with 50% methanol constant volume, the machine of treating is used.
With standard substance and sample difference sample introduction, the chromatograph of standard substance goes out peak figure and sees Fig. 1, and the appearance time of arbutin is about 6.8 minutes; The appearance time of gallic acid is about 7.3 minutes, and the appearance time of catechin is about 9.6 minutes, and the appearance time of chlorogenic acid is about 10.1 minutes; The appearance time of epicatechin is about 11.0 minutes, and caffeinic appearance time is about 11.5 minutes, and the appearance time of vanillin is about 12.7 minutes; The appearance time of ferulic acid is about 13.5 minutes; The rutin appearance time is about 14.4 minutes, and the phlorhizin appearance time is about 15.4 minutes, and the Quercetin appearance time is about 21.8 minutes.The chromatograph of sample goes out peak figure and sees Fig. 2.Can know that through calculating arbutin content is 96.66mg/100g in the sample, gallic acid content is 0.79mg/100g; Catechin content is 11.65mg/100g, and chlorogenic acid content is 7.84mg/100g, and epicatechin content is 2.79mg/100g; Caffeic acid content is 2.64mg/100g, and vanillin content is 4.45mg/100g, and ferulaic acid content is 1.90mg/100g; Rutin content is 1.64mg/100g, does not detect phlorhizin and Quercetin.The content of arbutin in testing sample is the highest; Be 74.1%; Explain that young fruit can be used as the natural resources that extract arbutin; The polyphenol purity of embodiment 5 pears polyphenol extracting solution is 88.7%, and " (liquid phase record the aldehydes matter content that summation/the FC method records of aldehydes matter) explains that this pears polyphenol extracting solution sample quality is better.
Claims (5)
1. a pears polyphenol extracting method is characterized in that pears young fruit peeling enucleation, is cut into less than 1cm
3Fritter, use the liquid nitrogen grinding powdered; Alcoholic solution with 30% ~ 90% carries out lixiviate to melonidum; The mass volume ratio of lixiviate sample and solution is 1:20 ~ 30; With constant temperature shaking table lucifuge, 50 ℃ ~ 70 ℃, at the uniform velocity lixiviate of 100 ~ 170rpm; Each extraction time is 2 ~ 6 hours, goes out supernatant with the centrifuge centrifugalize and is pears polyphenol extracting solution.
2. pears polyphenol extracting method according to claim 1 is characterized in that the alcoholic solution with 40% ~ 60% carries out lixiviate to melonidum.
3. pears polyphenol extracting method according to claim 1, the oscillation rate that it is characterized in that described constant temperature shaking table is 100 ~ 150rpm.
4. pears polyphenol extracting method according to claim 1 is characterized in that described extraction time is 2 ~ 4 hours.
5. pears polyphenol extracting method according to claim 1 is characterized in that described pears young fruit refers to behind the fallen flowers 1 ~ 2 month pear fruit.
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Cited By (4)
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| CN102940701A (en) * | 2012-12-11 | 2013-02-27 | 青岛海洋新材料科技有限公司 | Method for extracting pear polyphenol |
| WO2015100506A1 (en) * | 2013-12-31 | 2015-07-09 | Universidad De Talca | Extraction of phenolic compounds from fruit obtained from apple thinning |
| CN106361847A (en) * | 2016-11-07 | 2017-02-01 | 中国农业科学院郑州果树研究所 | Young pear fruit total phenol extracting method |
| CN109745374A (en) * | 2017-11-08 | 2019-05-14 | 大江生医股份有限公司 | Green pears young fruit extract is for reducing heavy metal in blood and the purposes of promotion lung function |
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| CN101756312A (en) * | 2009-12-11 | 2010-06-30 | 辽宁石油化工大学 | Method for preparing microencapsulated drink of Nanguo pear liver-protecting anti-alcohol agent |
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| CN101756312A (en) * | 2009-12-11 | 2010-06-30 | 辽宁石油化工大学 | Method for preparing microencapsulated drink of Nanguo pear liver-protecting anti-alcohol agent |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102940701A (en) * | 2012-12-11 | 2013-02-27 | 青岛海洋新材料科技有限公司 | Method for extracting pear polyphenol |
| WO2015100506A1 (en) * | 2013-12-31 | 2015-07-09 | Universidad De Talca | Extraction of phenolic compounds from fruit obtained from apple thinning |
| CN106361847A (en) * | 2016-11-07 | 2017-02-01 | 中国农业科学院郑州果树研究所 | Young pear fruit total phenol extracting method |
| CN106361847B (en) * | 2016-11-07 | 2019-06-11 | 中国农业科学院郑州果树研究所 | A kind of pears young fruit total phenol extracting method |
| CN109745374A (en) * | 2017-11-08 | 2019-05-14 | 大江生医股份有限公司 | Green pears young fruit extract is for reducing heavy metal in blood and the purposes of promotion lung function |
| CN109745374B (en) * | 2017-11-08 | 2021-09-10 | 百岳特生物科技（上海）有限公司 | Use of green pear fruit extract for reducing heavy metals in blood |
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Application publication date: 20121017 |