CN102973617B - A kind of extracting method of pomegranate peel polyphenol - Google Patents
A kind of extracting method of pomegranate peel polyphenol Download PDFInfo
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- CN102973617B CN102973617B CN201210530634.9A CN201210530634A CN102973617B CN 102973617 B CN102973617 B CN 102973617B CN 201210530634 A CN201210530634 A CN 201210530634A CN 102973617 B CN102973617 B CN 102973617B
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Abstract
An extracting method for pomegranate peel polyphenol, its step is as follows: by Pericarpium Granati rinsing, drying, be ground into after powder and cross 40 mesh sieves; Described Pomegranate Rind is joined in ethanol water, through microwave treatment; Again through water-bath backflow lixiviate, centrifugal 20min after sucking filtration, centrifugal power is 4000r/min, filters, and then rotary evaporation in vacuo reclaims ethanol, obtains polyphenolic extract; Described polyphenolic extract is formulated as the solution of 4mg/mL, flows through macroporous resin and adsorb, water-bath vibration 24h, bath temperature is 25 DEG C, and hunting power is 120r/min; By the resin filter after absorption, be filtered dry after distillation washing twice, carry out dynamic desorption with ethanol, concentration of alcohol is 40%, and eluent concentrates postlyophilization, obtains polyphenol extract.The method effectively can shorten extraction time, improves extraction ratio, improves purity.
Description
Technical field
The present invention relates to a kind of method extracting pomegranate peel polyphenol from Pericarpium Granati, platymiscium extracts field.
technical background
Pericarpium Granati is the dried peel of Punica granatum L., and property is sour, taste is astringent, and having the effectiveness of hemostasis, astringing intestine to stop diarrhea, parasite killing, is clinical conventional Chinese medicine.Pomegranate peel polyphenol is the general name that a class has polyphenol hydroxyl compound, comprise the multiple compounds such as Galla Turcica (Galla Helepensis) tannin, elladitannin, ellagic acid, chlorogenic acid, gallic acid, catechin, epicatechin, anthocyanidin, mainly be present in Pericarpium Granati, content is about 10 ~ 20% of its dry weight.In recent years, large quantity research shows, pomegranate peel polyphenol has free radical resisting, antimutagenic, aging resistance, antibacterial, angiocardiopathy preventing, improves the several functions such as climacteric syndrome, have in fields such as medicine, article of everyday use and food and act on widely, therefore, the method for inventing the high extraction pomegranate peel polyphenol of a kind of extraction efficiency has great importance.
In prior art, the extracting method of plant polyphenol mainly contains solution extraction, ultrasonic extraction, microwave method etc., but single extracting method productive rate is low.The present invention first adopts microwave extraction technique, destroys Pericarpium Granati cell, impels polyphenol substance stripping wherein and to external diffusion, then adopts alcohol steep, effectively can shorten extraction time, improve extraction ratio, improve purity.
Summary of the invention
The object of this invention is to provide a kind of method extracting pomegranate peel polyphenol from Pericarpium Granati, the method effectively can shorten extraction time, improves extraction ratio, improves purity.
For realizing above object, the extracting method of a kind of pomegranate peel polyphenol of the present invention, step is as follows:
(1) by Pericarpium Granati rinsing, drying, be ground into after powder and cross 40 mesh sieves;
(2) described Pomegranate Rind is joined in ethanol water, through microwave treatment;
(3) again through water-bath backflow lixiviate, centrifugal 20min after sucking filtration, centrifugal power is 4000r/min, filters, and then rotary evaporation in vacuo reclaims ethanol, obtains polyphenolic extract;
(4) described polyphenolic extract is formulated as the solution of 4mg/mL, flows through macroporous resin and adsorb, water-bath vibration 24h, bath temperature is 25 DEG C, and hunting power is 120r/min;
(5) by the resin filter after absorption, be filtered dry after distillation washing twice, carry out dynamic desorption with ethanol, concentration of alcohol is 40%, and eluent concentrates postlyophilization, obtains polyphenol extract.
Preferably, the concentration of alcohol described in step (2) is 30%-50%.
Preferably, the mass ratio of the Pomegranate Rind described in step (2) and ethanol is 1:20-1:30.
Preferably, the microwave power described in step (2) is 200-250W, and the microwave action time is 25-30s.
Preferably, the extraction temperature described in step (3) is 60-70 DEG C, and extracting times is 3-4 time, and extraction time is each 2-2.5h.
Preferably, the macroporous resin type described in step (4) is: HP-20, AB-8 or X-5, be more preferably HP-20.
Preferably, the polyphenolic extract described in step (4) flows through the flow velocity of macroporous resin is 3-4BV/h.
Preferably, the adsorption time described in step (4) is 2-3h.
Preferably, the elution rate described in step (5) is 2-3BV/h.
The method extracting pomegranate peel polyphenol from Pericarpium Granati of the present invention is the preferred experiment parameter obtained after many experiments, and each step all effectively can improve the extraction ratio of EFFECT OF POLYPHENOLIC EXTRACT FROM POMEGRANATE PEEL.
Water-soluble polyphenols is mainly distributed in the vacuole of cell, non-water-soluble Polyphenols compound is present on cell wall, and how to be combined with hydrogen bond formation with protein or polysaccharide compound, the ethanol of high concentration causes protein denaturation to be difficult to by water-soluble polyphenols lixiviate out, prevent the mass transport process of polyphenol compound, cause polyphenol content to reduce, therefore in step (2), concentration of alcohol is preferably 30%-50%.
When microwave power is 200-250W, best to the destructive power of cell, impel polyphenol substance stripping in Pericarpium Granati and to external diffusion, if continue to add high-power, the polyphenol degeneration of precipitation can be made, or with other component generation chemical reactions, cause extraction ratio to reduce.
Verify through many experiments, type be HP-20, AB-8 or X-5 macroporous resin to the static adsorption rate of pomegranate peel polyphenol and resolution factor all higher, can reach more than 85%, more preferred HP-20 type macroporous resin static adsorption rate and resolution factor are respectively 94.2%, 94.1%.
Embodiment
Embodiment 1:
Pomegranate peel polyphenol is extracted with following steps:
(1) by Pericarpium Granati rinsing, drying, be ground into after powder and cross 40 mesh sieves;
(2) described Pomegranate Rind being joined concentration is in the ethanol water of 30%, and the mass ratio of Pomegranate Rind and ethanol is 1:20, and through microwave treatment, microwave power is 250W, and the microwave action time is 25s;
(3) again through water-bath backflow lixiviate, extraction temperature is 70 DEG C, lixiviate 3 times, each 2.5h, centrifugal 20min after sucking filtration, and centrifugal power is 4000r/min, filters, and then rotary evaporation in vacuo reclaims ethanol, obtains polyphenolic extract;
Now measuring olive leaf polyphenol extraction ratio is 16.4%.
(4) described polyphenolic extract is formulated as the solution of 4mg/mL, flows through HP-20 type macroporous resin with the flow velocity of 3BV/h, absorption 2h, water-bath vibration 24h, hunting power is 120r/min;
(5) by the resin filter after absorption, be filtered dry after distillation washing twice, carry out dynamic desorption with ethanol, elution rate is 2BV/h, and concentration of alcohol is 40%, and eluent concentrates postlyophilization, obtains polyphenol extract.
The purity obtaining pomegranate peel polyphenol through above step is 75.8%.
Embodiment 2:
Pomegranate peel polyphenol is extracted with following steps:
(1) by Pericarpium Granati rinsing, drying, be ground into after powder and cross 40 mesh sieves;
(2) described Pomegranate Rind being joined concentration is in the ethanol water of 40%, and the mass ratio of Pomegranate Rind and ethanol is 1:30, and through microwave treatment, microwave power is 250W, and the microwave action time is 26s;
(3) again through water-bath backflow lixiviate, extraction temperature is 65 DEG C, lixiviate 4 times, each 2h, centrifugal 20min after sucking filtration, and centrifugal power is 4000r/min, filters, and then rotary evaporation in vacuo reclaims ethanol, obtains polyphenolic extract;
Now measuring olive leaf polyphenol extraction ratio is 16.6%.
(4) described polyphenolic extract is formulated as the solution of 4mg/mL, flows through HP-20 type macroporous resin with the flow velocity of 3.5BV/h, absorption 3h, water-bath vibration 24h, hunting power is 120r/min;
(5) by the resin filter after absorption, be filtered dry after distillation washing twice, carry out dynamic desorption with ethanol, elution rate is 2.5BV/h, and concentration of alcohol is 40%, and eluent concentrates postlyophilization, obtains polyphenol extract.
The purity obtaining pomegranate peel polyphenol through above step is 76.2%.
Embodiment 3:
Pomegranate peel polyphenol is extracted with following steps:
(1) by Pericarpium Granati rinsing, drying, be ground into after powder and cross 40 mesh sieves;
(2) described Pomegranate Rind being joined concentration is in the ethanol water of 50%, and the mass ratio of Pomegranate Rind and ethanol is 1:30, and through microwave treatment, microwave power is 250W, and the microwave action time is 28s;
(3) again through water-bath backflow lixiviate, extraction temperature is 60 DEG C, lixiviate 4 times, each 2.5h, centrifugal 20min after sucking filtration, and centrifugal power is 4000r/min, filters, and then rotary evaporation in vacuo reclaims ethanol, obtains polyphenolic extract;
Now measuring olive leaf polyphenol extraction ratio is 16.5%.
(4) described polyphenolic extract is formulated as the solution of 4mg/mL, flows through AB-8 type macroporous resin with the flow velocity of 4BV/h, absorption 3h, water-bath vibration 24h, hunting power is 120r/min;
(5) by the resin filter after absorption, be filtered dry after distillation washing twice, carry out dynamic desorption with ethanol, elution rate is 3BV/h, and concentration of alcohol is 40%, and eluent concentrates postlyophilization, obtains polyphenol extract.
The purity obtaining pomegranate peel polyphenol through above step is 73.3%.
Embodiment 4:
Pomegranate peel polyphenol is extracted with following steps:
(1) by Pericarpium Granati rinsing, drying, be ground into after powder and cross 40 mesh sieves;
(2) described Pomegranate Rind being joined concentration is in the ethanol water of 45%, and the mass ratio of Pomegranate Rind and ethanol is 1:30, and through microwave treatment, microwave power is 250W, and the microwave action time is 30s;
(3) again through water-bath backflow lixiviate, extraction temperature is 60 DEG C, lixiviate 4 times, each 2h, centrifugal 20min after sucking filtration, and centrifugal power is 4000r/min, filters, and then rotary evaporation in vacuo reclaims ethanol, obtains polyphenolic extract;
Now measuring olive leaf polyphenol extraction ratio is 16.1%.
(4) described polyphenolic extract is formulated as the solution of 4mg/mL, flows through X-5 type macroporous resin with the flow velocity of 4BV/h, absorption 3h, water-bath vibration 24h, hunting power is 120r/min;
(5) by the resin filter after absorption, be filtered dry after distillation washing twice, carry out dynamic desorption with ethanol, elution rate is 3BV/h, and concentration of alcohol is 40%, and eluent concentrates postlyophilization, obtains polyphenol extract.
The purity obtaining pomegranate peel polyphenol through above step is 73.7%.
Claims (6)
1. an extracting method for pomegranate peel polyphenol, is characterized in that: step is as follows:
(1) by Pericarpium Granati rinsing, drying, be ground into after powder and cross 40 mesh sieves;
(2) described Pomegranate Rind being joined volumetric concentration is in the ethanol water of 30%-50%, and through microwave treatment, described microwave power is 200-250W, and the microwave action time is 25-30s;
(3) again through water-bath backflow lixiviate, centrifugal 20min after sucking filtration, centrifugal power is 4000r/min, filters, and then rotary evaporation in vacuo reclaims ethanol, and obtain polyphenolic extract, extraction temperature is 60-70 DEG C, and extracting times is 3-4 time, and extraction time is each 2-2.5h;
(4) described polyphenolic extract is formulated as the solution of 4mg/mL, flows through macroporous resin and adsorb, water-bath vibration 24h, bath temperature is 25 DEG C, and hunting power is 120r/min, and described macroporous resin type is: HP-20 or X-5;
(5) by the resin filter after absorption, be filtered dry after distillation washing twice, carry out dynamic desorption with ethanol, concentration of alcohol is 40%, and eluent concentrates postlyophilization, obtains polyphenol extract.
2. the extracting method of a kind of pomegranate peel polyphenol as described in claim 1, is characterized in that: the mass ratio of the Pomegranate Rind described in step (2) and ethanol is 1:20-1:30.
3. the extracting method of a kind of pomegranate peel polyphenol as claimed in claim 1, is characterized in that: the macroporous resin type described in step (4) is: HP-20.
4. the extracting method of a kind of pomegranate peel polyphenol as claimed in claim 1, is characterized in that: the flow velocity that the polyphenolic extract described in step (4) flows through macroporous resin is 3-4BV/h.
5. the extracting method of a kind of pomegranate peel polyphenol as claimed in claim 1, is characterized in that: the adsorption time described in step (4) is 2-3h.
6. the extracting method of a kind of pomegranate peel polyphenol as claimed in claim 1, is characterized in that: the elution rate described in step (5) is 2-3BV/h.
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| CN103204885B (en) * | 2013-04-02 | 2015-12-23 | 吉林大学 | A kind of rapid extraction separation method of corn filament polyphenol |
| CN105878306A (en) * | 2016-04-11 | 2016-08-24 | 浙江中医药大学 | Preparation method of pomegranate peel polyphenols |
| CN106063828B (en) * | 2016-06-20 | 2019-11-26 | 武汉市农业科学院 | A kind of oil extracting method of tree peony blade polyphenol |
| CN106619873B (en) * | 2016-12-29 | 2020-05-05 | 华宝香精股份有限公司 | HPEF extraction method for improving antioxidant activity of papaya peel polyphenol |
| CN106860490A (en) * | 2016-12-30 | 2017-06-20 | 浙江海洋大学 | A kind of preparation technology of the pomegranate peel polyphenol of anti-fatigue active |
| CN109706047A (en) * | 2019-03-08 | 2019-05-03 | 四川轻化工大学 | Preparation method of anoectochilus roxburghii health-care wine |
| CN113717139A (en) * | 2021-09-15 | 2021-11-30 | 耒阳市刘燕酿制生物科技有限公司 | Method for extracting quercetin from pomegranate peel |
| CN114632042A (en) * | 2022-03-24 | 2022-06-17 | 仙婷(广州)科技研发有限公司 | Liposome containing pomegranate polyphenol extract and application thereof |
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| CN102755360A (en) * | 2012-07-24 | 2012-10-31 | 西华大学 | Method for extracting pomegranate peel polyphenols from pomegranate peel |
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