CN104784246A - Method for extracting protodioscin from fenugreek seeds - Google Patents
Method for extracting protodioscin from fenugreek seeds Download PDFInfo
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- CN104784246A CN104784246A CN201510182283.0A CN201510182283A CN104784246A CN 104784246 A CN104784246 A CN 104784246A CN 201510182283 A CN201510182283 A CN 201510182283A CN 104784246 A CN104784246 A CN 104784246A
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- semen trigonellae
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Abstract
The invention discloses a method for extracting protodioscin from fenugreek seeds. The method comprises the following the steps: (1) pressing the fenugreek seeds with a screw-type oil expeller; taking off lipid compositions to obtain fenugreek seed cake meal; (2) extracting the fenugreek seed cake meal with purified water twice, filtering the extracting solution to obtain filtrates; combining the filtrates; (3) conducting purification on the combined filtrate with a CAD-40 macroporous resin column, carrying out washing with water, using ethyl alcohol with a concentration of 70% for elution, carrying out decompressing and concentrating till no alcohol exists, and carrying out spraying and drying to obtain an extraction containing protodioscin. The method for extracting protodioscin from the fenugreek seeds is simple in extracting operation, and low in energy consumption and cost, and has the advantage that the purity of effective components in the extraction can be improved.
Description
Technical field
The present invention relates to a kind of method extracting protodioscin, particularly relate to a kind of method extracting protodioscin from Semen Trigonellae seed.
Background technology
Protodioscin belongs to steroidal saponin, and protodioscin has sexual function improving, blood fat reducing, has the effects such as poisoning and leukemia to cancerous cell.
Patent application document CN 102670697 A discloses a kind of preparation method of Semen Trigonellae water extract, comprises the following steps: (1) gets Semen Trigonellae seed, adds the water of 10 times of weight, soaks 20-30 minute, boils 20-30 minute, take out and retain filtrate; (2) in filtering residue, add the water of 8 times amount again, soak 20-30 minute, boil 20-30 minute, retain filtrate; (3) merge 2 filtrates, drying with water bath is powder, obtained Semen Trigonellae water extract.
Protodioscin content in the Semen Trigonellae water extract of above-mentioned preparation is low, and yield is low, and impurity is many, and impact uses effect, and production cost is high.
Summary of the invention
The object of the present invention is to provide a kind of method extracting protodioscin from Semen Trigonellae seed, have extraction simple to operate, energy consumption is little, and cost is low, and can improve the purity of the effective ingredient in extract.
For solving the problems of the technologies described above, a kind of method extracting protodioscin from Semen Trigonellae seed of the present invention, the method comprises the steps:
(1) Semen Trigonellae seed screw oil expeller is squeezed, slough lipid components, obtain Semen Trigonellae seedcake Hectometer;
(2) by Semen Trigonellae seedcake Hectometer purified water lixiviate 2 times, extracting liquid filtering obtains filtrate, merging filtrate;
(3) filtrate after merging is carried out purification with CAD-40 macroporous adsorptive resins, washing, 70% ethanol elution, is evaporated to without alcohol, spraying dry, obtains the extract containing protodioscin.
Semen Trigonellae seed screw oil expeller is squeezed, sloughs lipid components, obtain Semen Trigonellae seedcake Hectometer, can be easy to remove liposoluble constituent, reduce impurity content, be convenient to the carrying out of subsequent extracted technique, can leaching process be simplified, and the method K cryogenic treatment, energy-conserving and environment-protective.Semen Trigonellae seed makes protodioscin effective ingredient more easily separate out after squeezing into cake Hectometer, improve the response rate.With purified water lixiviate Semen Trigonellae seedcake Hectometer, greatly can reduce costs, and prevent fat-soluble impurity from separating out, simplify purification step.Adopt CAD-40 macroporous adsorbent resin dynamic adsorption technology, can obtain the higher unit adsorbance of protodioscin and good desorption efficiency, can prepare the protodioscin of high-quality, can shorten the production cycle, equipment needed thereby is simple.Eluent, by being evaporated to without alcohol, can reclaiming ethanol, reduce costs.Concentrated solution spraying dry obtains the extract containing protodioscin, can simplify the forming steps of product, be applicable to suitability for industrialized production.
As preferably, in described step (1), pressing temperature is 10 ~ 40 DEG C, and squeeze pressure is 10 ~ 40MPa.
As preferably, in described step (2), each consumption of purified water is 6 ~ 8 times of Semen Trigonellae seedcake Hectometer, and extraction temperature is 20 ~ 50 DEG C, and extraction time is each 1 ~ 2 hour.
As preferably, in described step (3), the flow velocity of filtrate macroporous adsorptive resins purification is 0.5 ~ 2BV/h, and resin demand is made a living 3 ~ 6 times of dose, and resin column blade diameter length ratio is 1:1 ~ 5.
As preferably, in described step (3), the consumption of the purified water of cleaning resin column is 1 ~ 3BV, and the cleaning flow velocity of purified water is 2 ~ 4BV/h.
As preferably, in described step (3), alcoholic solution consumption is 1 ~ 2BV, and the elution flow rate of alcoholic solution is 2 ~ 4BV/h.
As preferably, in described step (3), concentrating under reduced pressure temperature is 50 ~ 60 DEG C, and concentrating under reduced pressure pressure is-0.07 ~-0.09MPa.
As preferably, in described step (3), spray drying condition is: nebulizer frequency conversion is adjusted to 20Hz, and inlet temperature is 180 DEG C, leaving air temp is 90 DEG C, after spray tower runs 2 hours, exhaust blower frequency conversion is adjusted to 32Hz, nebulizer frequency conversion is adjusted to 36Hz, runs 30 minutes.
A kind of effective effect extracting the method for protodioscin from Semen Trigonellae seed of the present invention is: whole extraction process is simple, energy-conserving and environment-protective, energy consumption is little, cost is low, workable, production equipment requires low, is applicable to suitability for industrialized production, and can improve the purity of the effective ingredient in extract, in extract, protodioscin content reaches more than 50%.
Detailed description of the invention
Below in conjunction with specific embodiment, embodiment of the present invention are described in detail.Should be appreciated that enforcement of the present invention is not limited to the following examples, any pro forma accommodation make the present invention and/or change all will fall into protection scope of the present invention.
Embodiment 1
Squeezed by 100kg Semen Trigonellae seed screw oil expeller, pressing temperature is 10 DEG C, and squeeze pressure is 40MPa, sloughs lipid components, obtains Semen Trigonellae seedcake Hectometer.Semen Trigonellae seedcake Hectometer 6 times of purified water are carried out lixiviate, and extraction temperature is 50 DEG C, and extraction time is 1 hour, and extracting liquid filtering is obtained filtrate, with purified water in the above described manner again lixiviate once, merging filtrate.Merging filtrate is carried out purification with the flow velocity CAD-40 macroporous adsorptive resins of 1BV/h, wherein resin demand is made a living 3 times of dose, resin column blade diameter length ratio is 1:1, then resin column is cleaned by the purified water of 1BV with 4BV/h flow velocity, then use 70% ethanol of 1BV with 4BV/h flow velocity eluting, collect eluent, eluent is evaporated to without alcohol, concentrating under reduced pressure temperature is 60 DEG C, concentrating under reduced pressure pressure is-0.07MPa, reclaim ethanol, concentrated solution carries out spraying dry, nebulizer frequency conversion is adjusted to 20Hz, inlet temperature is 180 DEG C, leaving air temp is 90 DEG C, after spray tower runs 2 hours, exhaust blower frequency conversion is adjusted to 32Hz, nebulizer frequency conversion is adjusted to 36Hz, run 30 minutes, obtain the extract 5.22kg containing protodioscin, wherein the content of protodioscin is 52.4%.
Embodiment 2
Squeezed by 100kg Semen Trigonellae seed screw oil expeller, pressing temperature is 25 DEG C, and squeeze pressure is 25MPa, sloughs lipid components, obtains Semen Trigonellae seedcake Hectometer.Semen Trigonellae seedcake Hectometer 7 times of purified water are carried out lixiviate, and extraction temperature is 35 DEG C, and extraction time is 2 hours, and extracting liquid filtering is obtained filtrate, with purified water in the above described manner again lixiviate once, merging filtrate.Merging filtrate is carried out purification with the flow velocity CAD-40 macroporous adsorptive resins of 0.5BV/h, wherein resin demand is made a living 6 times of dose, resin column blade diameter length ratio is 1:5, then resin column is cleaned by the purified water of 2BV with 2BV/h flow velocity, then use 70% ethanol of 1.5BV with 2BV/h flow velocity eluting, collect eluent, eluent is evaporated to without alcohol, concentrating under reduced pressure temperature is 55 DEG C, concentrating under reduced pressure pressure is-0.08MPa, reclaim ethanol, concentrated solution carries out spraying dry, nebulizer frequency conversion is adjusted to 20Hz, inlet temperature is 180 DEG C, leaving air temp is 90 DEG C, after spray tower runs 2 hours, exhaust blower frequency conversion is adjusted to 32Hz, nebulizer frequency conversion is adjusted to 36Hz, run 30 minutes, obtain the extract 5.08kg containing protodioscin, wherein the content of protodioscin is 54.7%.
Embodiment 3
Squeezed by 100kg Semen Trigonellae seed screw oil expeller, pressing temperature is 40 DEG C, and squeeze pressure is 10MPa, sloughs lipid components, obtains Semen Trigonellae seedcake Hectometer.Semen Trigonellae seedcake Hectometer 8 times of purified water are carried out lixiviate, and extraction temperature is 20 DEG C, and extraction time is 2 hours, and extracting liquid filtering is obtained filtrate, with purified water in the above described manner again lixiviate once, merging filtrate.Merging filtrate is carried out purification with the flow velocity CAD-40 macroporous adsorptive resins of 2BV/h, wherein resin demand is made a living 4 times of dose, resin column blade diameter length ratio is 1:3, then resin column is cleaned by the purified water of 3BV with 3BV/h flow velocity, then use 70% ethanol of 2BV with 3BV/h flow velocity eluting, collect eluent, eluent is evaporated to without alcohol, concentrating under reduced pressure temperature is 50 DEG C, concentrating under reduced pressure pressure is-0.09MPa, reclaim ethanol, concentrated solution carries out spraying dry, nebulizer frequency conversion is adjusted to 20Hz, inlet temperature is 180 DEG C, leaving air temp is 90 DEG C, after spray tower runs 2 hours, exhaust blower frequency conversion is adjusted to 32Hz, nebulizer frequency conversion is adjusted to 36Hz, run 30 minutes, obtain the extract 5.28kg containing protodioscin, wherein the content of protodioscin is 51.8%.
Claims (8)
1. extract a method for protodioscin from Semen Trigonellae seed, it is characterized in that: the method comprises the steps:
(1) Semen Trigonellae seed screw oil expeller is squeezed, slough lipid components, obtain Semen Trigonellae seedcake Hectometer;
(2) by Semen Trigonellae seedcake Hectometer purified water lixiviate 2 times, extracting liquid filtering obtains filtrate, merging filtrate;
(3) filtrate after merging is carried out purification with CAD-40 macroporous adsorptive resins, washing, 70% ethanol elution, is evaporated to without alcohol, spraying dry, obtains the extract containing protodioscin.
2. the method extracting protodioscin from Semen Trigonellae seed according to claim 1, is characterized in that: in described step (1), pressing temperature is 10 ~ 40 DEG C, and squeeze pressure is 10 ~ 40MPa.
3. the method extracting protodioscin from Semen Trigonellae seed according to claim 1, it is characterized in that: in described step (2), each consumption of purified water is 6 ~ 8 times of Semen Trigonellae seedcake Hectometer, extraction temperature is 20 ~ 50 DEG C, and extraction time is each 1 ~ 2 hour.
4. the method extracting protodioscin from Semen Trigonellae seed according to claim 1, it is characterized in that: in described step (3), the flow velocity of filtrate macroporous adsorptive resins purification is 0.5 ~ 2BV/h, resin demand is made a living 3 ~ 6 times of dose, and resin column blade diameter length ratio is 1:1 ~ 5.
5. the method extracting protodioscin from Semen Trigonellae seed according to claim 1, is characterized in that: in described step (3), the consumption of the purified water of cleaning resin column is 1 ~ 3BV, and the cleaning flow velocity of purified water is 2 ~ 4BV/h.
6. the method extracting protodioscin from Semen Trigonellae seed according to claim 1, is characterized in that: in described step (3), alcoholic solution consumption is 1 ~ 2BV, and the elution flow rate of alcoholic solution is 2 ~ 4BV/h.
7. the method extracting protodioscin from Semen Trigonellae seed according to claim 1, is characterized in that: in described step (3), concentrating under reduced pressure temperature is 50 ~ 60 DEG C, and concentrating under reduced pressure pressure is-0.07 ~-0.09MPa.
8. the method extracting protodioscin from Semen Trigonellae seed according to claim 1, it is characterized in that: in described step (3), spray drying condition is: nebulizer frequency conversion is adjusted to 20Hz, inlet temperature is 180 DEG C, leaving air temp is 90 DEG C, after spray tower runs 2 hours, exhaust blower frequency conversion is adjusted to 32Hz, nebulizer frequency conversion is adjusted to 36Hz, runs 30 minutes.
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| CN201510182283.0A CN104784246A (en) | 2015-04-17 | 2015-04-17 | Method for extracting protodioscin from fenugreek seeds |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110117232A (en) * | 2018-02-07 | 2019-08-13 | 内蒙古昶辉生物科技股份有限公司 | The extracting method of effective component in faenum graecum seed |
| CN110117231A (en) * | 2018-02-07 | 2019-08-13 | 内蒙古昶辉生物科技股份有限公司 | A method of extracting 4-hydroxyisoleucine and total saposins from faenum graecum seed |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101255183A (en) * | 2008-03-11 | 2008-09-03 | 南昌大学 | Method for extracting protodioscin from semen trigonellae |
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2015
- 2015-04-17 CN CN201510182283.0A patent/CN104784246A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101255183A (en) * | 2008-03-11 | 2008-09-03 | 南昌大学 | Method for extracting protodioscin from semen trigonellae |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110117232A (en) * | 2018-02-07 | 2019-08-13 | 内蒙古昶辉生物科技股份有限公司 | The extracting method of effective component in faenum graecum seed |
| CN110117231A (en) * | 2018-02-07 | 2019-08-13 | 内蒙古昶辉生物科技股份有限公司 | A method of extracting 4-hydroxyisoleucine and total saposins from faenum graecum seed |
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