CN102935101A - Extraction method of olive leaf polyphenol - Google Patents
Extraction method of olive leaf polyphenol Download PDFInfo
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- CN102935101A CN102935101A CN2012105267931A CN201210526793A CN102935101A CN 102935101 A CN102935101 A CN 102935101A CN 2012105267931 A CN2012105267931 A CN 2012105267931A CN 201210526793 A CN201210526793 A CN 201210526793A CN 102935101 A CN102935101 A CN 102935101A
- Authority
- CN
- China
- Prior art keywords
- folium olive
- polyphenol
- extracting method
- folium
- olive polyphenol
- 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.)
- Granted
Links
- 240000007817 Olea europaea Species 0.000 title claims abstract description 71
- 150000008442 polyphenolic compounds Chemical class 0.000 title claims abstract description 67
- 235000013824 polyphenols Nutrition 0.000 title claims abstract description 67
- 238000000605 extraction Methods 0.000 title claims abstract description 21
- 235000002725 Olea europaea Nutrition 0.000 title abstract 4
- 238000000034 method Methods 0.000 claims abstract description 31
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 24
- 239000011347 resin Substances 0.000 claims abstract description 21
- 229920005989 resin Polymers 0.000 claims abstract description 21
- 238000000874 microwave-assisted extraction Methods 0.000 claims abstract description 18
- 239000000287 crude extract Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 21
- 239000000843 powder Substances 0.000 claims description 21
- 239000000284 extract Substances 0.000 claims description 15
- 239000012153 distilled water Substances 0.000 claims description 14
- 238000001179 sorption measurement Methods 0.000 claims description 9
- 239000012141 concentrate Substances 0.000 claims description 7
- 238000003795 desorption Methods 0.000 claims description 7
- 238000004821 distillation Methods 0.000 claims description 7
- 239000003480 eluent Substances 0.000 claims description 7
- 238000010828 elution Methods 0.000 claims description 7
- 238000011010 flushing procedure Methods 0.000 claims description 7
- 239000007788 liquid Substances 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 238000010521 absorption reaction Methods 0.000 claims 1
- 238000011017 operating method Methods 0.000 claims 1
- 238000009777 vacuum freeze-drying Methods 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract 1
- 230000018044 dehydration Effects 0.000 abstract 1
- 238000006297 dehydration reaction Methods 0.000 abstract 1
- 238000000926 separation method Methods 0.000 abstract 1
- 241000196324 Embryophyta Species 0.000 description 4
- 238000002474 experimental method Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009792 diffusion process Methods 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 241001529246 Platymiscium Species 0.000 description 1
- 230000003064 anti-oxidating effect Effects 0.000 description 1
- 230000000259 anti-tumor effect Effects 0.000 description 1
- 239000003963 antioxidant agent Substances 0.000 description 1
- 230000003078 antioxidant effect Effects 0.000 description 1
- ZYGHJZDHTFUPRJ-UHFFFAOYSA-N benzo-alpha-pyrone Natural products C1=CC=C2OC(=O)C=CC2=C1 ZYGHJZDHTFUPRJ-UHFFFAOYSA-N 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 235000001671 coumarin Nutrition 0.000 description 1
- 150000004775 coumarins Chemical class 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007850 degeneration Effects 0.000 description 1
- 230000001066 destructive effect Effects 0.000 description 1
- 235000013325 dietary fiber Nutrition 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 229930003935 flavonoid Natural products 0.000 description 1
- 150000002215 flavonoids Chemical class 0.000 description 1
- 235000017173 flavonoids Nutrition 0.000 description 1
- -1 lignanoids Chemical class 0.000 description 1
- 210000004185 liver Anatomy 0.000 description 1
- 235000015097 nutrients Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 235000009048 phenolic acids Nutrition 0.000 description 1
- 150000007965 phenolic acids Chemical class 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 229930000044 secondary metabolite Natural products 0.000 description 1
- PJANXHGTPQOBST-UHFFFAOYSA-N stilbene Chemical class C=1C=CC=CC=1C=CC1=CC=CC=C1 PJANXHGTPQOBST-UHFFFAOYSA-N 0.000 description 1
- 235000018553 tannin Nutrition 0.000 description 1
- 229920001864 tannin Polymers 0.000 description 1
- 239000001648 tannin Substances 0.000 description 1
- 238000002137 ultrasound extraction Methods 0.000 description 1
Landscapes
- Medicines Containing Plant Substances (AREA)
Abstract
The invention relates to an extraction method of olive leaf polyphenol. The method comprises the following steps: with water as a solvent, obtaining olive leaf polyphenol crude extract by adopting microwave extraction, then carrying out macroporous resin separation, pressure reduction and concentration, and vacuum freeze dehydration to obtain the olive leaf polyphenol. The method is characterized in that the the microwave power is increased for every other 20-60s in the microwave extraction process. The method has the beneficial effects that the use amount of the solvent can be reduced, the extraction yield is increased, and the purity is improved.
Description
Technical field
The present invention relates to a kind of method of extracting the Folium olive polyphenol from Folium olive, platymiscium extracts the field.
Technical background
Plant polyphenol is the important secondary metabolite that extensively is present in the plant; be distributed widely in root, leaf, skin, sarcocarp and the shell of plant; have the different physiological roles such as antioxidation, antitumor, the liver protecting; be the antioxidant that human body must absorb from food every day, be called as the 7th nutrient after dietary fiber.By structure polyphenol is divided into following a few class: simple phenols (C
6), lignanoids, Coumarins, stilbene class (C
6-C
2-C
6), flavonoid (C
6-C
1-C
6, C
6-C
3-C
6), phenolic acids (C
6-C
1, C
6-C
3) and the chemical compound such as tannin class.
In the 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 replaces traditional organic solvent with water, adopts simultaneously improved microwave extraction technique, destroys the Folium olive cell, impel wherein the polyphenol substance stripping and to external diffusion, can reduce the consumption of solvent, improve extraction ratio, improve purity.
Summary of the invention
The purpose of this invention is to provide a kind of method of extracting the Folium olive polyphenol from Folium olive, the method can reduce the consumption of solvent, improves extraction ratio, improves purity.
For realizing above purpose, the extracting method of a kind of Folium olive polyphenol of the present invention, step is as follows:
(1) with Folium olive flushing, dry, cross 40 mesh sieves after being ground into powder;
(2) described Folium olive powder is joined in the distilled water, the mass ratio of Folium olive powder and distilled water is 1:20-1:40, through microwave extraction, design temperature is 80 ℃, in microwave power is the scope of 100-300W, improve a microwave power every 20-60s, dry extraction liquid obtains Folium olive polyphenol crude extract;
Preferably, microwave extraction technique is 120W, 160W, 200W, 240W, 280W for setting gradually microwave power every 20s.
Preferably, microwave extraction technique is 150W, 200W, 250W for setting gradually microwave power every 40s.
Preferably, microwave extraction technique is 170W, 230W for setting gradually microwave power every 60s.
(3) described polyphenol crude extract is added the solution that water is made into 10mg/mL, flowing through macroporous resin adsorbs, flow velocity is 3-4BV/h, the macroporous resin type is selected HP-20, AB-8 or X-5, adsorption time is 2-3h, then water-bath vibration 24h, bath temperature is 25 ℃, hunting power is 120r/min;
(4) be filtered dry behind the resin filter after will adsorbing, twice of distillation washing, carry out dynamic desorption with ethanol, elution rate is 2-3BV/h, and concentration of alcohol is 40%, and eluent concentrates postlyophilization, obtains polyphenol extract.
The method of extracting the Folium olive polyphenol from Folium olive of the present invention is the preferred experiment parameter that obtains behind many experiments, and each step all can effectively improve the extraction ratio of Folium olive polyphenol extract.
When microwave power is 100-300W, best to the destructive power of cell, impel in the Folium olive polyphenol substance stripping and to external diffusion, if continue to add high-power, can make the polyphenol degeneration of separating out, or with other component generation chemical reactions, cause extraction ratio to reduce.Particularly, according to the variation of polyphenol concentration in the solution, in above-mentioned range of microwave power, improve a microwave power every 20-60s, increase gradually the destruction dynamics to cell, can make to greatest extent the polyphenol substance stripping, therefore can significantly improve extraction ratio.
Verify through many experiments, type is that the macroporous resin of HP-20, AB-8 or X-5 is all higher to static adsorption rate and the resolution factor of Folium olive polyphenol, 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:
Extract the Folium olive polyphenol with following steps:
(1) with Folium olive flushing, dry, cross 40 mesh sieves after being ground into powder;
(2) described Folium olive powder is joined in the distilled water, the mass ratio of Folium olive powder and distilled water is 1:20, through microwave extraction, design temperature is 80 ℃, setting gradually microwave power every 20s is 120W, 160W, 200W, 240W, 280W, then dry extraction liquid obtains Folium olive polyphenol crude extract;
Measure Folium olive polyphenol extraction ratio this moment is 18.2%.
(3) described polyphenol crude extract is added the solution that water is made into 10mg/mL, flow through HP-20 type macroporous resin and adsorb, flow velocity is 3BV/h, and adsorption time is 2h, water-bath vibration 24h then, and bath temperature is 25 ℃, hunting power is 120r/min;
(4) be filtered dry behind the resin filter after will adsorbing, twice of distillation washing, 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 that obtains the Folium olive polyphenol through above step is 74.2%.
Embodiment 2:
Extract the Folium olive polyphenol with following steps:
(1) with Folium olive flushing, dry, cross 40 mesh sieves after being ground into powder;
(2) described Folium olive powder is joined in the distilled water, the mass ratio of Folium olive powder and distilled water is 1:20, through microwave extraction, design temperature is 80 ℃, setting gradually microwave power every 40s is 150W, 200W, 250W, then dry extraction liquid obtains Folium olive polyphenol crude extract;
Measure Folium olive polyphenol extraction ratio this moment is 18.9%.
(3) described polyphenol crude extract is added the solution that water is made into 10mg/mL, flow through HP-20 type macroporous resin and adsorb, flow velocity is 4BV/h, and adsorption time is 3h, water-bath vibration 24h then, and bath temperature is 25 ℃, hunting power is 120r/min;
(4) be filtered dry behind the resin filter after will adsorbing, twice of distillation washing, 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 that obtains the Folium olive polyphenol through above step is 75.1%.
Embodiment 3:
Extract the Folium olive polyphenol with following steps:
(1) with Folium olive flushing, dry, cross 40 mesh sieves after being ground into powder;
(2) described Folium olive powder is joined in the distilled water, the mass ratio of Folium olive powder and distilled water is 1:20, through microwave extraction, design temperature is 80 ℃, setting gradually microwave power every 60s is 170W, 230W, and then dry extraction liquid obtains Folium olive polyphenol crude extract;
Measure Folium olive polyphenol extraction ratio this moment is 17.4%.
(3) described polyphenol crude extract is added the solution that water is made into 10mg/mL, flow through AB-8 type macroporous resin and adsorb, flow velocity is 4BV/h, and adsorption time is 3h, water-bath vibration 24h then, and bath temperature is 25 ℃, hunting power is 120r/min;
(4) be filtered dry behind the resin filter after will adsorbing, twice of distillation washing, 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 that obtains the Folium olive polyphenol through above step is 73.5%.
Embodiment 4:
Extract the Folium olive polyphenol with following steps:
(1) with Folium olive flushing, dry, cross 40 mesh sieves after being ground into powder;
(2) described Folium olive powder is joined in the distilled water, the mass ratio of Folium olive powder and distilled water is 1:30, through microwave extraction, design temperature is 80 ℃, setting gradually microwave power every 40s is 150W, 200W, 250W, then dry extraction liquid obtains Folium olive polyphenol crude extract;
Measure Folium olive polyphenol extraction ratio this moment is 18.6%.
(3) described polyphenol crude extract is added the solution that water is made into 10mg/mL, flow through X-5 type macroporous resin and adsorb, flow velocity is 4BV/h, and adsorption time is 3h, water-bath vibration 24h then, and bath temperature is 25 ℃, hunting power is 120r/min;
(4) be filtered dry behind the resin filter after will adsorbing, twice of distillation washing, 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 that obtains the Folium olive polyphenol through above step is 73.3%.
Embodiment 5:
Extract the Folium olive polyphenol with following steps:
(1) with Folium olive flushing, dry, cross 40 mesh sieves after being ground into powder;
(2) described Folium olive powder is joined in the distilled water, the mass ratio of Folium olive powder and distilled water is 1:40, through microwave extraction, design temperature is 80 ℃, setting gradually microwave power every 40s is 150W, 200W, 250W, then dry extraction liquid obtains Folium olive polyphenol crude extract;
Measure Folium olive polyphenol extraction ratio this moment is 18.1%.
(3) described polyphenol crude extract is added the solution that water is made into 10mg/mL, flow through X-5 type macroporous resin and adsorb, flow velocity is 3.5BV/h, and adsorption time is 3h, water-bath vibration 24h then, and bath temperature is 25 ℃, hunting power is 120r/min;
(4) be filtered dry behind the resin filter after will adsorbing, twice of distillation washing, 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 that obtains the Folium olive polyphenol through above step is 73.5%.
Claims (10)
1. the extracting method of a Folium olive polyphenol, take water as solvent, adopt microwave extraction to obtain Folium olive polyphenol crude extract, then separate by macroporous resin, obtain the Folium olive polyphenol behind concentrating under reduced pressure, the vacuum freeze-drying, it is characterized in that: microwave extraction technique is for improving a microwave power every 20-60s.
2. the extracting method of a kind of Folium olive polyphenol as claimed in claim 1, it is characterized in that: operating procedure is:
With Folium olive flushing, dry, cross 40 mesh sieves after being ground into powder;
Described Folium olive powder is joined in the distilled water, and through microwave extraction, design temperature is 80 ℃, and dry extraction liquid obtains Folium olive polyphenol crude extract;
Described polyphenol crude extract is added the solution that water is made into 10mg/mL, flow through macroporous resin and adsorb, water-bath vibration 24h, bath temperature is 25 ℃, hunting power is 120r/min;
With the resin filter after the absorption, distillation is filtered dry after washing twice, carries out dynamic desorption with ethanol, and concentration of alcohol is 40%, and eluent concentrates postlyophilization, obtains polyphenol extract.
3. the extracting method of a kind of Folium olive polyphenol as claimed in claim 1 or 2, it is characterized in that: described microwave power is 100-300W.
4. the extracting method of a kind of Folium olive polyphenol as claimed in claim 3 is characterized in that: described microwave extraction technique is 120W, 160W, 200W, 240W, 280W for setting gradually microwave power every 20s.
5. the extracting method of a kind of Folium olive polyphenol as claimed in claim 3 is characterized in that: described microwave extraction technique is 150W, 200W, 250W for setting gradually microwave power every 40s.
6. the extracting method of a kind of Folium olive polyphenol as claimed in claim 3 is characterized in that: described microwave extraction technique is 170W, 230W for setting gradually microwave power every 60s.
7. a kind of extracting method of Folium olive polyphenol as described in claim 2, it is characterized in that: the mass ratio of the Folium olive powder described in the step (2) and distilled water is 1:20-1:40.
8. the extracting method of a kind of Folium olive polyphenol as claimed in claim 1 or 2, it is characterized in that: described macroporous resin type is: HP-20, AB-8 or X-5.
9. the extracting method of a kind of Folium olive polyphenol as claimed in claim 2, it is characterized in that: the flow velocity that the polyphenolic extract described in the step (3) flows through macroporous resin is 3-4BV/h, and adsorption time is 2-3h.
10. the extracting method of a kind of Folium olive polyphenol as claimed in claim 2, it is characterized in that: the elution rate described in the step (4) is 2-3BV/h.
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| CN201210526793.1A CN102935101B (en) | 2012-12-10 | 2012-12-10 | A kind of extracting method of olive leaf polyphenol |
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| CN201210526793.1A CN102935101B (en) | 2012-12-10 | 2012-12-10 | A kind of extracting method of olive leaf polyphenol |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104490977A (en) * | 2014-11-28 | 2015-04-08 | 桂林市和胤祥新型材料有限公司 | Method for extracting olive polyphenol from olive leaves |
| CN106617060A (en) * | 2016-12-27 | 2017-05-10 | 云南中烟工业有限责任公司 | Fructus phyllanthi polyphenols enriching and purifying method |
| CN106924398A (en) * | 2017-02-28 | 2017-07-07 | 广西南岜仔科技有限公司 | Longan seed polyphenol extracting method |
| CN107019738A (en) * | 2017-02-28 | 2017-08-08 | 广西南岜仔科技有限公司 | A kind of hypoglycemic longan seed polyphenol extracting method |
| CN107308033A (en) * | 2017-05-22 | 2017-11-03 | 福建省亚热带植物研究所 | A kind of preparation method of olive fruits high-purity polyphenol and its application in cosmetics |
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| CN102273623A (en) * | 2011-05-20 | 2011-12-14 | 西华大学 | Preparation method of olive leaf extract |
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2012
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Patent Citations (2)
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| CN102273623A (en) * | 2011-05-20 | 2011-12-14 | 西华大学 | Preparation method of olive leaf extract |
| CN102617655A (en) * | 2012-03-12 | 2012-08-01 | 江南大学 | Method for subcritical water extraction of oleuropein |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104490977A (en) * | 2014-11-28 | 2015-04-08 | 桂林市和胤祥新型材料有限公司 | Method for extracting olive polyphenol from olive leaves |
| CN106617060A (en) * | 2016-12-27 | 2017-05-10 | 云南中烟工业有限责任公司 | Fructus phyllanthi polyphenols enriching and purifying method |
| CN106924398A (en) * | 2017-02-28 | 2017-07-07 | 广西南岜仔科技有限公司 | Longan seed polyphenol extracting method |
| CN107019738A (en) * | 2017-02-28 | 2017-08-08 | 广西南岜仔科技有限公司 | A kind of hypoglycemic longan seed polyphenol extracting method |
| CN107308033A (en) * | 2017-05-22 | 2017-11-03 | 福建省亚热带植物研究所 | A kind of preparation method of olive fruits high-purity polyphenol and its application in cosmetics |
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| CN102935101B (en) | 2016-02-03 |
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