CN106336441A - Extraction process of high-purity phloridzin - Google Patents
Extraction process of high-purity phloridzin Download PDFInfo
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- CN106336441A CN106336441A CN201510391682.8A CN201510391682A CN106336441A CN 106336441 A CN106336441 A CN 106336441A CN 201510391682 A CN201510391682 A CN 201510391682A CN 106336441 A CN106336441 A CN 106336441A
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Abstract
The invention discloses an extraction process of high-purity phloridzin. The process includes the steps of: (1) stock solution extraction: adding water that is 8 times the amount of a phloridzin-containing mashed raw material into the same, conducting soaking for 3h, performing heating to boiling, maintaining slight boiling for 2h to obtain an extracted solution; adding purified water that is 6 times the amount of residue into the same and performing heating to boiling, maintaining slight boiling for 2h to obtain a secondary extracted solution; merging the extracted solutions, carrying out cooling and filtering, and collecting the filtrate; (2) preliminary extraction of a finished product: subjecting the filtrate to adsorption by macroporous resin D101, controlling the column pass flow at 80L/H, using 20-50degree ethanol to conduct gradient elution, performing fractional collection on the outflow solution, carrying out vacuum concentration, standing and cooling, conducting crystal precipitation at 0-4DEG C, and carrying out high-speed centrifugal dehydration; and (3) finished product extraction: conducting pure water redissolution, vacuum concentration, recrystallization, high-speed centrifugal dehydration and drying, thus obtaining a finished product. The extraction process of high-purity phloridzin provided by the invention has easily available raw materials, not only solves the environmental problem, but also improves the product yield, and greatly reduces the cost, and has the advantages of simple reaction process, convenient operation and no pollution.
Description
Technical field
The present invention relates to a kind of phlorhizin extraction process, particularly to a kind of high-purity phlorizin extraction process, belong to phlorhizin extractive technique field.
Background technology
Phlorhizin is widely present in various plants, it is primarily present in rosaceous plant such as apple tree, in other plants, content is low, phlorhizin is one of apple tree aldehydes matter, research data shows, phlorhizin accounts for 95% of aldehydes matter total content in apple tree, and initial phlorhizin is exactly to extract to obtain from the branch of apple tree, bark and leaveves.At present, the method extracting phlorhizin has resin adsorption method, polyamide chromatography post separation method and extraction, wherein, resin adsorption method adsorption capacity is big, and selectivity is good it is easy to desorption, high mechanical strength, Regeneration Treatment be simple, adsorption rate is fast, and it is free from environmental pollution, but the focus of the toxicity problem of the perforating agent used in macroporous resin preparation process, always technique dispute, it becomes the obstacle using macroporous adsorption resin technology separation phlorhizin；Using polyamide chromatography post separation method is simple to operate, good separating effect, safety, and load capacity is high, non-specific adsorption is few, and the method is disadvantageous in that in elution process using having the methanol of medium toxic action to human body as eluant；Methanol affects very greatly on the nervous system of human body and blood system, and it is taken in human body through digestive tract, respiratory tract or skin and all can produce toxic reaction；Extraction is during extracting phlorhizin, employ and less ethanol and ethyl acetate are poisoned to human body, but ethanol is used in purge process as extractant, and ethanol has paralysis effect to human nerve, in view of safety problem, it is very difficult to apply in medicine and food；Therefore the extraction of phlorhizin is also needed to study new technique.
Content of the invention
(1) technical problem to be solved
For solving the above problems, the present invention proposes a kind of high-purity phlorizin extraction process it is ensured that low production cost, can reduce environmental pollution, and good product quality.
(2) technical scheme
The high-purity phlorizin extraction process of the present invention, described technique comprises the steps:
(1) stock solution is extracted: the raw material mashed containing phlorhizin adds 8 times of pure water, soaks 3 hours, be heated to boiling, keep micro-boiling 2 hours, obtain extracting solution；6 times of pure water of residue is heated to boiling, and keeps micro-boiling 2 hours, obtains secondary raffinate. united extraction liquid, cooling, filter, collection filtrate:
(2) tentatively extract finished product: filtrate adsorbs through macroporous resin d101, crossing column flow is 80l/h, with 20 °～50 ° of ethanol gradient elution, by effluent Fractional Collections, concentrated in vacuo, standing, cooling, 0～4 DEG C separates out crystallization, and high speed centrifugation is dehydrated；
(3) finished product extracts: pure water returns molten, concentrated in vacuo, recrystallization, and high speed centrifugation is dehydrated, and is dried, obtains finished product.
As preferred embodiment, the described raw material mashed is squeezed the juice waste material for 3% Fructus Mali pumilae for water content.
As preferred embodiment, described raw material is skin, root and the branch and leaf of rosaceous plant.
Beneficial effect
Compared with prior art, the high-purity phlorizin extraction process of the present invention, has the advantage that
1st, using the skin of cheap rosaceous plant, root and branch and leaf it is also possible to extract phlorhizin from discarded waste material of squeezing the juice, raw material is easy to get this technique, not only solve environmental problem, and improve the yield of product, substantially reduce cost, course of reaction is simple, easy to operate, environmentally safe.
2nd, this technique extraction process is simple, and power consumption is low, while simplifying production technology, reduces production cost.
3rd, this technique mainly adopts Aqua pure extract, is that the residual quantity of hazardous solvent in raw material is preferably minimized, and meets country to food and pharmaceutical raw material requirement, reduces organic residue, improves yield.
Brief description
Fig. 1 is the production technological process of the present invention.
Specific embodiment
Embodiment 1:
As shown in figure 1, high-purity phlorizin extraction process of the present invention, described technique comprises the steps:
(1) stock solution is extracted: water content is that 3% Fructus Mali pumilae is squeezed the juice waste material, adds 8 times of pure water, soak 3 hours, be heated to boiling that holding micro-boiling 2 hours obtains extracting solution；6 times of pure water of residue is heated to boiling, and keeps micro-boiling 2 hours, obtains secondary raffinate. united extraction liquid, cooling, filter, collection filtrate:
(2) tentatively extract finished product: filtrate adsorbs through macroporous resin d101, crossing column flow is 80l/h, with 20 °～50 ° of ethanol gradient elution, by effluent Fractional Collections, concentrated in vacuo, standing, cooling, 0～4 DEG C separates out crystallization, and high speed centrifugation is dehydrated；
(3) finished product extracts: pure water returns molten, concentrated in vacuo, recrystallization, and high speed centrifugation is dehydrated, and is dried, obtains finished product.
This technique squeezes the juice waste material for raw material using Fructus Mali pumilae; by extraction process; realize the preparation of phlorhizin; preparation cost is in 600 yuan/kilogram; there is obvious cost advantage than other technique of the prior art; realize inexpensive, pollution-free, three wastes and prepare with scale phlorhizin, it is easy to accomplish 5 tons/year of scale, gained phlorhizin purity is more than 98.0%.
Embodiment 2:
As shown in figure 1, high-purity phlorizin extraction process of the present invention, described technique comprises the steps:
(1) stock solution is extracted: the skin of the rosaceous plant mashed, root and branch and leaf adds 8 times of pure water, soaks 3 hours, be heated to boiling, keep micro-boiling 2 hours, obtain extracting solution；6 times of pure water of residue is heated to boiling, and keeps micro-boiling 2 hours, obtains secondary raffinate. united extraction liquid, cooling, filter, collection filtrate:
(2) tentatively extract finished product: filtrate adsorbs through macroporous resin d101, crossing column flow is 80l/h, with 20 °～50 ° of ethanol gradient elution, by effluent Fractional Collections, concentrated in vacuo, standing, cooling, 0～4 DEG C separates out crystallization, and high speed centrifugation is dehydrated；
(3) finished product extracts: pure water returns molten, concentrated in vacuo, recrystallization, and high speed centrifugation is dehydrated, and is dried, obtains finished product.
Embodiment described above is only that the preferred embodiment of the present invention is described, and not the spirit and scope of the present invention is defined.On the premise of without departing from design concept of the present invention; various modifications and improvement that this area ordinary person makes to technical scheme; protection scope of the present invention all should be dropped into, the technology contents that the present invention is claimed, all record in detail in the claims.
Claims (3)
1. a kind of high-purity phlorizin extraction process is it is characterised in that described technique comprises the steps:
(1) stock solution is extracted: the raw material mashed containing phlorhizin adds 8 times of pure water, soaks 3 hours, be heated to boiling, keep micro-boiling 2 hours, obtain extracting solution；6 times of pure water of residue is heated to boiling, and keeps micro-boiling 2 hours, obtains secondary raffinate. united extraction liquid, cooling, filter, collection filtrate:
(2) tentatively extract finished product: filtrate adsorbs through macroporous resin d101, crossing column flow is 80l/h, with 20 °～50 ° of ethanol gradient elution, by effluent Fractional Collections, concentrated in vacuo, standing, cooling, 0～4 DEG C separates out crystallization, and high speed centrifugation is dehydrated；
(3) finished product extracts: pure water returns molten, concentrated in vacuo, recrystallization, and high speed centrifugation is dehydrated, and is dried, obtains finished product.
2. the high-purity phlorizin extraction process according to claim 1 it is characterised in that: the described raw material mashed is squeezed the juice waste material for 3% Fructus Mali pumilae for water content.
3. the high-purity phlorizin extraction process according to claim 1 it is characterised in that: described raw material is the skin of rosaceous plant, root and branch and leaf.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510391682.8A CN106336441A (en) | 2015-07-07 | 2015-07-07 | Extraction process of high-purity phloridzin |
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| CN201510391682.8A CN106336441A (en) | 2015-07-07 | 2015-07-07 | Extraction process of high-purity phloridzin |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109503683A (en) * | 2018-12-03 | 2019-03-22 | 三峡大学 | The isolation and purification method of phloridzin in a kind of Malus spectabilis Aqueous extracts |
| CN109535208A (en) * | 2018-12-27 | 2019-03-29 | 大理大学 | The method of phloridzin is prepared from M. rockii |
| CN111393491A (en) * | 2020-05-07 | 2020-07-10 | 江西省科学院应用化学研究所 | Method for green preparation of high-purity phlorizin from wild Jinchai |
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| CN1683382A (en) * | 2005-03-11 | 2005-10-19 | 天津市尖峰天然产物研究开发有限公司 | Process for extracting phlorhizin from bark, root, branch and leaf of rosaceous plant and juice pressing waste material |
| CN101392008A (en) * | 2007-09-18 | 2009-03-25 | 兴化格林生物制品有限公司 | Extraction technique of high-purity phlorizin |
| 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 |
| CN104098623A (en) * | 2014-07-21 | 2014-10-15 | 神农架聚能药业有限公司 | Method for extracting phloridzin of malus hupehensis (pamp.) rehd |
| CN104592323A (en) * | 2014-12-26 | 2015-05-06 | 中国农业科学院农产品加工研究所 | Dual-aqueous phase extracting method of phloridzin from apple residues |
| 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 |
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2015
- 2015-07-07 CN CN201510391682.8A patent/CN106336441A/en active Pending
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1683382A (en) * | 2005-03-11 | 2005-10-19 | 天津市尖峰天然产物研究开发有限公司 | Process for extracting phlorhizin from bark, root, branch and leaf of rosaceous plant and juice pressing waste material |
| CN101392008A (en) * | 2007-09-18 | 2009-03-25 | 兴化格林生物制品有限公司 | Extraction technique of high-purity phlorizin |
| 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 |
| 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 |
| CN104098623A (en) * | 2014-07-21 | 2014-10-15 | 神农架聚能药业有限公司 | Method for extracting phloridzin of malus hupehensis (pamp.) rehd |
| CN104592323A (en) * | 2014-12-26 | 2015-05-06 | 中国农业科学院农产品加工研究所 | Dual-aqueous phase extracting method of phloridzin from apple residues |
| 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 |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN109503683A (en) * | 2018-12-03 | 2019-03-22 | 三峡大学 | The isolation and purification method of phloridzin in a kind of Malus spectabilis Aqueous extracts |
| CN109535208A (en) * | 2018-12-27 | 2019-03-29 | 大理大学 | The method of phloridzin is prepared from M. rockii |
| CN111393491A (en) * | 2020-05-07 | 2020-07-10 | 江西省科学院应用化学研究所 | Method for green preparation of high-purity phlorizin from wild Jinchai |
| CN111393491B (en) * | 2020-05-07 | 2023-04-07 | 江西省科学院应用化学研究所 | Method for green preparation of high-purity phlorizin from wild Jinchai |
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