CN101392008A - Extraction technique of high-purity phlorizin - Google Patents
Extraction technique of high-purity phlorizin Download PDFInfo
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- CN101392008A CN101392008A CNA2007101323946A CN200710132394A CN101392008A CN 101392008 A CN101392008 A CN 101392008A CN A2007101323946 A CNA2007101323946 A CN A2007101323946A CN 200710132394 A CN200710132394 A CN 200710132394A CN 101392008 A CN101392008 A CN 101392008A
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Abstract
The invention discloses an extraction process of a high purity phlorizin, comprising the following steps: (1) the raw materials are added with 4-8 times pure water, marinated for 1-3 hours, heated to boiling and micro boiling is kept for 2-3 hours so as to obtain an extracting solution; residue is heated to boiling by using 2-6 times pure water and micro boiling is kept for 2-3 hours so as to obtain a secondary extracting solution; the extracting solutions are merged, cooled and filtered and then the filtered liquid is collected; (2) the filtered liquid is adsorbed by macroporous resin and subjected to gradient elution by using 20 DEG and 50 DEG ethanol; the effluent liquid is collected in subsection, concentrated in vacuum, placed in a quiescence way and cooled, dissolves out crystal at 0-4 DEG C, and dehydrates by high-speed centrifugation; and (3) re-dissolving of pure water, vacuum concentration, re-crystallization, high-speed centrifugation dehydration and drying are carried out so as to obtain the finished product. By adopting pure water for extraction, the organic-residue is decreased and simultaneously the product content is more than 99 percent.
Description
Technical field
The present invention relates to a kind of extraction process of natural phant effective ingredient, particularly relate to and a kind ofly cover bark, root, the branches and leaves of section plant and the waste material of squeezing the juice is a raw material, extract the technology of phlorizin with rose.
Background technology
Phlorizin belongs to the plant polyphenol compounds.External more for the research of phlorizin relevant physiological function.Phlorizin can activate the cellular protein expression kinases, and the unordered hyperplasia of pair cell has restraining effect, is a kind of antimutagenic factor, can be used for the assisting therapy of skin liver cancer and other tumours.Phlorizin content dependency (Shinohara1998) studies show that phlorizin can effectively slow down the proliferate of colon cancer cell and liver neoplasm cell; Extremely strong antioxygen is arranged, to greasy anti-oxidant concentration between 10-30ppm; Phlorizin has remarkable step-down, effect for reducing fat, is described as by the people to be the natural depressor ＂ of ＂, and is particularly suitable for hypertensive patient or hyperlipidemia patient; The phlorizin external application can stop carbohydrate content to enter epidermic cell, thereby suppresses the excessive secretion of cutaneous gland, the vigorous type acne of treatment secretion; Phlorizin can suppress the melanocyte activity, and various skin splashs are had desalination effect etc.(1998) such as Kanda of Japan confirm that the ＂ phlorizin ＂ that extracts can effectively suppress the free and hyaluronic activity of histamine from immature green apple, play antianaphylactic effect, in addition, anti-dental caries, reducing cholesterol and the effect of preventing and treating cardiovascular disorder all have report.Phlorizin since its unique physiologically active and health-care effect in recent years in America and Europe's fields such as foodstuffs industry, cosmetic industry and medicine industry; A kind of situation of selling well healthcare products have been become.At present, current phlorizin production technique is to adopt ethanol extraction method, and its technical process is: raw material (fruit tree branch, pomace etc.) is added ethanol, soak, be heated to boiling, filter, concentrate, reclaim ethanol to filtered liquid and do not have the alcohol flavor, filtered liquid is through macroporous resin adsorption, ethanol gradient elution with 20%, 40%, 60%, 80% with the effluent liquid Fractional Collections, concentrates, use chloroform extraction, abandon chloroform layer, reconcentration to proportion is 1-1.08,1-4 ℃ of crystallization separated out, and be centrifugal, the dry finished product that gets.This technical process complexity, the cost height, owing to adopted the organic solvent chloroform, production process has certain danger, and product is organic residual, and content is low, and quality is bad.
Summary of the invention
Purpose of the present invention is in order to overcome existing technical process complexity, the cost height, have residually, and problem such as content is low provides a kind of new extraction process, this technology not only makes technical process simplify, production cost reduces, and can also reduce the organic residual of product, improves the quality of product, the product content height reaches more than 99%.
Technical scheme of the present invention is summarized as follows:
The extraction process of high-purity phlorizin comprises the steps: that (1) adds 4-8 pure water doubly with raw material, soaks 1-3 hour, is heated to and boils, and keeps little and boils 2-3 hour, gets extracting solution; Residue is heated to 2-6 pure water doubly and boils, and keeps little and boils 2-3 hour, gets secondary raffinate, united extraction liquid, and cooling is filtered, and collects filtered liquid; (2) filtered liquid is through macroporous resin adsorption, and with 20 °, 50 ° ethanol gradient elution, with the effluent liquid Fractional Collections, vacuum concentration leaves standstill, and cooling is separated out crystallization for 0-4 ℃, the high speed centrifugation dehydration; (3) pure water return molten, vacuum concentration, recrystallize, high speed centrifugation dehydration, drying, finished product.
Described raw material is that apple or pears or peach or cherry or other rose cover the edible plants of section.
Described step (1): the pure water with 4 times of raw material addings, soaked 1-3 hour, be heated to and boil, keep little and boiled 2-3 hour, get extracting solution; Residue with 3 times pure water be heated to and boil, keep little and boiled 2-3 hour, secondary raffinate, united extraction liquid, cooling is filtered, and collects filtered liquid.
The post flow excessively of described macroporous resin adsorption is 80-100L/H.
Described macroporous resin can be AB-8, can be D101, also can be ADS-7.
Advantage of the present invention is:
(1), can adopt cheap rose to cover skin, root and the branches and leaves of section plant, even from depleted is squeezed the juice waste material, extract phlorizin, raw material is easy to get, and turns waste into wealth.
(2), extraction process is simple, it is low to consume energy, and when simplifying production technique, has reduced production cost.
(3), the main pure water that adopts extracts in technological process, makes the less residue of hazardous solvent in the raw material, meets the requirement of country to food and medicine, has reduced organic residually, has improved product content.
Embodiment
The present invention is further illustrated below in conjunction with specific embodiment.
Embodiment 1
A kind of extraction process of high-purity phlorizin comprises the steps: that (1) is that the 3% apple waste material of squeezing the juice adds 8 times pure water with water content, soaks 3 hours, is heated to and boils, and keeps little and boils 2 hours, must extracting solution; Residue is heated to 6 times pure water and boils, keep little and boiled 2 hours, secondary raffinate, united extraction liquid, cooling is filtered, and collects filtered liquid; (2) filtered liquid is through macroporous resin D101 absorption, and crossing the post flow is 80L/H, and with 20 °, 50 ° ethanol gradient elution, with the effluent liquid Fractional Collections, vacuum concentration leaves standstill, and cooling is separated out crystallization for 0-4 ℃, the high speed centrifugation dehydration; (3) pure water return molten, vacuum concentration, recrystallize, high speed centrifugation dehydration, drying, finished product.
Embodiment 2
A kind of extraction process of high-purity phlorizin comprises the steps: that (1) is that the 1% apple waste material of squeezing the juice adds 7 times pure water with water content, soaks 2 hours, is heated to and boils, and keeps little and boils 3 hours, must extracting solution; Residue is heated to 5 times pure water and boils, keep little and boiled 2 hours, secondary raffinate, united extraction liquid, cooling is filtered, and collects filtered liquid; (2) filtered liquid is through macroporous resin AB-8 absorption, and crossing the post flow is 85L/H, and with 20 °, 50 ° ethanol gradient elution, with the effluent liquid Fractional Collections, vacuum concentration leaves standstill, and cooling is separated out crystallization for 0-4 ℃, the high speed centrifugation dehydration; (3) pure water return molten, vacuum concentration, recrystallize, high speed centrifugation dehydration, drying, finished product.
Embodiment 3
A kind of extraction process of high-purity phlorizin comprises the steps: that (1) is that 3% the pears waste material of squeezing the juice adds 4 times pure water with water content, soaks 1 hour, is heated to and boils, and keeps little and boils 3 hours, must extracting solution; Residue is heated to 6 times pure water and boils, keep little and boiled 2 hours, secondary raffinate, united extraction liquid, cooling is filtered, and collects filtered liquid; (2) filtered liquid is through macroporous resin ADS-7 absorption, and crossing the post flow is 90L/H, and with 20 °, 50 ° ethanol gradient elution, with the effluent liquid Fractional Collections, vacuum concentration leaves standstill, and cooling is separated out crystallization for 0-4 ℃, the high speed centrifugation dehydration; (3) pure water return molten, vacuum concentration, recrystallize, high speed centrifugation dehydration, drying, finished product.
Embodiment 4
A kind of extraction process of high-purity phlorizin comprises the steps: that (1) is that 3% the peach waste material of squeezing the juice adds 6 times pure water with water content, soaks 1 hour, is heated to and boils, and keeps little and boils 3 hours, must extracting solution; Residue is heated to 4 times pure water and boils, keep little and boiled 3 hours, secondary raffinate, united extraction liquid, cooling is filtered, and collects filtered liquid; (2) filtered liquid is through macroporous resin AB-8 absorption, and crossing the post flow is 95L/H, and with 20 °, 50 ° ethanol gradient elution, with the effluent liquid Fractional Collections, vacuum concentration leaves standstill, and cooling is separated out crystallization for 0-4 ℃, the high speed centrifugation dehydration; (3) pure water return molten, vacuum concentration, recrystallize, high speed centrifugation dehydration, drying, finished product.
Embodiment 5
A kind of extraction process of high-purity phlorizin comprises the steps: that (1) is that 2 the cherry waste material of squeezing the juice adds 6 times pure water with water content, soaks 2 hours, is heated to and boils, and keeps little and boils 2 hours, must extracting solution; Residue is heated to 5 times pure water and boils, keep little and boiled 3 hours, secondary raffinate, united extraction liquid, cooling is filtered, and collects filtered liquid; (2) filtered liquid is through macroporous resin ADS-7 absorption, and crossing the post flow is 100L/H, and with 20 °, 50 ° ethanol gradient elution, with the effluent liquid Fractional Collections, vacuum concentration leaves standstill, and cooling is separated out crystallization for 0-4 ℃, the high speed centrifugation dehydration; (3) pure water return molten, vacuum concentration, recrystallize, high speed centrifugation dehydration, drying, finished product.
Embodiment 6
A kind of extraction process of high-purity phlorizin comprises the steps: that (1) cut segment about salty 1cm with spray, adds 6 times pure water, soaks 2 hours, is heated to and boils, keep little and boiled 2 hours, extracting solution; Residue is heated to 4 times pure water and boils, keep little and boiled 3 hours, secondary raffinate, united extraction liquid, cooling is filtered, and collects filtered liquid; (2) filtered liquid is through macroporous resin ADS-7 absorption, and crossing the post flow is 100L/H, and with 20 °, 50 ° ethanol gradient elution, with the effluent liquid Fractional Collections, vacuum concentration leaves standstill, and cooling is separated out crystallization for 0-4 ℃, the high speed centrifugation dehydration; (3) pure water return molten, vacuum concentration, recrystallize, high speed centrifugation dehydration, drying, finished product.
Embodiment 7
Rose can be covered the bark of section plant or root and the immature vegetables and fruits in the fruit planting process is that raw material extracts phlorizin by the step of above-mentioned several embodiment.
Claims (5)
1, the extraction process of high-purity phlorizin comprises the steps: that (1) adds 4-8 pure water doubly with raw material, soaks 1-3 hour, is heated to and boils, and keeps little and boils 2-3 hour, gets extracting solution; Residue is heated to 2-6 pure water doubly and boils, and keeps little and boils 2-3 hour, gets secondary raffinate, united extraction liquid, and cooling is filtered, and collects filtered liquid; (2) filtered liquid is through macroporous resin adsorption, and with 20 °, 50 ° ethanol gradient elution, with the effluent liquid Fractional Collections, vacuum concentration leaves standstill, and cooling is separated out crystallization for 0-4 ℃, the high speed centrifugation dehydration; (3) pure water return molten, vacuum concentration, recrystallize, high speed centrifugation dehydration, drying, finished product.
2, the extraction process of high-purity phlorizin according to claim 1 is characterized in that: described raw material is that apple or pears or peach or cherry or other rose cover the edible plants of section.
3, the extraction process of high-purity phlorizin according to claim 1 and 2 is characterized in that: described step (1): the pure water with 4 times of raw material addings, soaked 1-3 hour, and be heated to and boil, keep little and boiled 2-3 hour, get extracting solution; Residue with 3 times pure water be heated to and boil, keep little and boiled 2-3 hour, secondary raffinate, united extraction liquid, cooling is filtered, and collects filtered liquid.
4, the extraction process of high-purity phlorizin according to claim 1 and 2 is characterized in that: the post flow excessively of described macroporous resin adsorption is 80-100L/H.
5, the extraction process of high-purity phlorizin according to claim 1 and 2 is characterized in that: described macroporous resin can be AB-8, can be D101, also can be ADS-7.
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| Application Number | Priority Date | Filing Date | Title |
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| CNA2007101323946A CN101392008A (en) | 2007-09-18 | 2007-09-18 | Extraction technique of high-purity phlorizin |
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| CNA2007101323946A CN101392008A (en) | 2007-09-18 | 2007-09-18 | Extraction technique of high-purity phlorizin |
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Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811949A (en) * | 2010-05-14 | 2010-08-25 | 上海利盛生化有限公司 | Purification method of phloretin powder |
| CN102086220A (en) * | 2010-12-31 | 2011-06-08 | 广州市天吻娇颜化妆品有限公司 | Extraction and purification method of phlorizin in litchi peels |
| CN102643315A (en) * | 2012-04-17 | 2012-08-22 | 陕西嘉禾植物化工有限责任公司 | Method for purifying phlorizin from apple velamen |
| CN103214530A (en) * | 2013-03-29 | 2013-07-24 | 陕西工业职业技术学院 | Separation and purification method for phlorizin in apple pomace |
| CN103626811A (en) * | 2013-10-24 | 2014-03-12 | 恩施市锦华生物工程有限责任公司 | Method for extracting and separating high-purity phlorizin from Cynomorium songaricum |
| CN104045671A (en) * | 2013-03-16 | 2014-09-17 | 永州一东生物技术有限责任公司 | Method for extracting and purifying phlorizin in apple root-bark |
| CN104610394A (en) * | 2015-01-30 | 2015-05-13 | 望宏端 | Method for extracting phlorizin with different purity from twigs and green leaves of Malus hupehensis |
| CN105777822A (en) * | 2016-04-17 | 2016-07-20 | 中国农业科学院郑州果树研究所 | Method for preparing high-purity phloridzin by virtue of apple tree branches |
| CN105924482A (en) * | 2016-04-29 | 2016-09-07 | 中南林业科技大学 | Method for extracting phloretin from camellia oleifera leaves |
| CN106336441A (en) * | 2015-07-07 | 2017-01-18 | 天津优利果蔬食品有限公司 | Extraction process of high-purity phloridzin |
| CN107602638A (en) * | 2017-09-27 | 2018-01-19 | 三原利华生物技术有限公司 | The method that phloridzin is prepared using apple branches and leaves, root skin |
-
2007
- 2007-09-18 CN CNA2007101323946A patent/CN101392008A/en active Pending
Cited By (17)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101811949B (en) * | 2010-05-14 | 2013-06-05 | 上海利盛生化有限公司 | Purification method of phloretin powder |
| CN101811949A (en) * | 2010-05-14 | 2010-08-25 | 上海利盛生化有限公司 | Purification method of phloretin powder |
| CN102086220A (en) * | 2010-12-31 | 2011-06-08 | 广州市天吻娇颜化妆品有限公司 | Extraction and purification method of phlorizin in litchi peels |
| CN102643315A (en) * | 2012-04-17 | 2012-08-22 | 陕西嘉禾植物化工有限责任公司 | Method for purifying phlorizin from apple velamen |
| CN102643315B (en) * | 2012-04-17 | 2014-11-05 | 陕西嘉禾植物化工有限责任公司 | Method for purifying phlorizin from apple velamen |
| CN104045671A (en) * | 2013-03-16 | 2014-09-17 | 永州一东生物技术有限责任公司 | Method for extracting and purifying phlorizin in apple root-bark |
| CN103214530A (en) * | 2013-03-29 | 2013-07-24 | 陕西工业职业技术学院 | Separation and purification method for phlorizin in apple pomace |
| CN103214530B (en) * | 2013-03-29 | 2015-12-02 | 陕西工业职业技术学院 | The separation purification method of phlorizin in a kind of apple residue |
| CN103626811B (en) * | 2013-10-24 | 2016-04-06 | 恩施市锦华生物工程有限责任公司 | A kind of method of extraction and isolation phlorizin from cynomorium songaricum |
| CN103626811A (en) * | 2013-10-24 | 2014-03-12 | 恩施市锦华生物工程有限责任公司 | Method for extracting and separating high-purity phlorizin from Cynomorium songaricum |
| CN104610394A (en) * | 2015-01-30 | 2015-05-13 | 望宏端 | Method for extracting phlorizin with different purity from twigs and green leaves of Malus hupehensis |
| CN106336441A (en) * | 2015-07-07 | 2017-01-18 | 天津优利果蔬食品有限公司 | Extraction process of high-purity phloridzin |
| CN105777822A (en) * | 2016-04-17 | 2016-07-20 | 中国农业科学院郑州果树研究所 | Method for preparing high-purity phloridzin by virtue of apple tree branches |
| CN105777822B (en) * | 2016-04-17 | 2019-07-12 | 中国农业科学院郑州果树研究所 | A method of phloridzin is prepared using apple branch |
| CN105924482A (en) * | 2016-04-29 | 2016-09-07 | 中南林业科技大学 | Method for extracting phloretin from camellia oleifera leaves |
| CN107602638A (en) * | 2017-09-27 | 2018-01-19 | 三原利华生物技术有限公司 | The method that phloridzin is prepared using apple branches and leaves, root skin |
| CN107602638B (en) * | 2017-09-27 | 2021-03-02 | 三原利华生物技术有限公司 | Method for preparing phlorizin by using apple branches, leaves and root barks |
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