CN103054915A - Novel production process for total flavones of hippophae rhamnoides - Google Patents
Novel production process for total flavones of hippophae rhamnoides Download PDFInfo
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- CN103054915A CN103054915A CN2012105953349A CN201210595334A CN103054915A CN 103054915 A CN103054915 A CN 103054915A CN 2012105953349 A CN2012105953349 A CN 2012105953349A CN 201210595334 A CN201210595334 A CN 201210595334A CN 103054915 A CN103054915 A CN 103054915A
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Abstract
The invention discloses a novel production process for total flavones of hippophae rhamnoides. The process comprises the steps as follows: washing raw materials; adding into a feeding hopper; rotating a mainframe of an extraction tank set; enabling materials to be fed into the front end of the extraction tank set backwardly and slowly; at the same time, enabling extracting solvents to enter into extraction tanks from a liquid inlet pipe at the tail end of the extraction tank set, penetrate through the moving materials from the rear ends of the tanks and flow to the front ends; and enabling the solid phase materials and the liquid phase materials to be fully contacted in the inverse motion so as to extract effective ingredients from the medicinal materials. Dregs are forcedly conveyed to a discharge hole for discharge through a discharge conveyer and squeezed by a special squeezer to squeeze out residual liquor in the dregs from the tissues of the medicinal materials so as to reduce the content of the residual liquor in the dregs. The extraction efficiency is higher and the extraction process is safer. The macroporous adsorption resin and the silica column chromatography for purification are selected and used at the same time, so that the separation effect is better. The finished total flavones of hippophae rhamnoides with the highest yield of 2% and the content of more than 70% can be obtained.
Description
Technical field:
The invention belongs to the natural organic chemistry field, relate to a kind of production technology of Fructus Hippophae total flavones, particularly relate to a kind of production new technique that utilizes countercurrent extraction, macroporous adsorbent resin coupling silica gel column chromatography purification Fructus Hippophae total flavones.
Background technology:
Fructus Hippophae Hippophae rhamnoides Linn, another name vinegar willow, yellow acid thorn, acid thorn willow, black thorn, acid thorn are the fruit of Elaeangnaceae hippophae plant Fructus Hippophae.Contain sea buckthorn fruit and contain flavones ingredient isorhamnetin (isorhamnetin), isorhamnetin-3-O-β-D-Glucose glycoside (isorham-netin-3-O-β-D-glucoside), isorhamnetin-3-O-β-rutinoside (isorhamnetin-3-O-β-rutinoside), globulariacitrin (rutin), astragalin (astragalin) and Quercetin (quercetin) and nimbecetin (kaempferol) are the low glucoside of glycoside unit.Also contain vitamin (vitamin) A, B1, B2, C, E, dehydroascorbic acid (dehydroascorbic acid), folic acid (folic acid), carotene (carotene), carotenoid (carotenoid), cachou extract (catechin), anthocyanidin (anthocyanin) etc. have the effect of relieving cough and resolving phlegm, invigorating the stomach and promoting digestion, promoting blood circulation to remove blood stasis.
Fructus Hippophae total flavones has cough-relieving, relievings asthma and eliminate the phlegm, expand the usefulness of coronary vasodilator, cholesterol reducing, is usually used in treating ischemic heart desease, and treatment angina pectoris effective percentage is reached 94%.In recent years, it is found that in the fruit of large right plant Fructus Hippophae and contain a large amount of Fructus Hippophae total flavoness, because its raw material Fructus Hippophae source is wider, therefrom extract Fructus Hippophae total flavones and obtained encouraging progress, name is called just to disclose in the patent application of " safe extraction technology of general flavone from whole sea-buckthorn fruit " sea-buchthorn fresh fruit is obtained natural juice and peel with the distinct methods extractive technique of separation and purification total flavones respectively after squeezing.Fructus Hippophae total flavones extraction process in the above-mentioned patent documentation mainly is through obtaining natural juice and peel after the squeezing, front natural juice obtains intermediate through separation, filter pressing, hybrid extraction, rear peel obtains intermediate through the processing of vibration sorting sieve, separation, hybrid extraction, intermediate is obtained flavone through the defat of non-ethers solvent, precipitation, oven dry, although last Fructus Hippophae total flavones purity is very high, but its technique itself expends greatly, and practical application effect is nothing like the effect of countercurrent extraction, the separation of macroporous adsorbent resin coupling silica gel column chromatography.
Summary of the invention
The object of the invention is to provide a kind of production new technique of Fructus Hippophae total flavones; The object of the invention also be to provide a kind of convenient and swift, raw material sources abundant, extraction efficiency is high, separation and purification successful, the production technology of utilizing Continuous Countercurrent Extraction and enriching and purifying macroporous resin Fructus Hippophae total flavones that dna purity is high.
The present invention seeks to be achieved through the following technical solutions.
A kind of production new technique of Fructus Hippophae total flavones, its step is as follows:
(1) Fructus Hippophae is cleaned the rear continuous countercurrent extracting tank ethanol water reflux, extract, that adds;
(2) extracting liquid filtering that will process through (1) gets the Fructus Hippophae total flavones crude extract;
(3) gained Fructus Hippophae total flavones crude extract is concentrated, get the thick concentrated solution of Fructus Hippophae total flavones;
(4) with the thick concentrated solution thin up of gained Fructus Hippophae total flavones, and filter, get filtrate;
(5) with the upper broad spectrum type macroporous resin adsorption post of gained filtrate, adsorb the complete impurity that washes with water, use again the ethanol aqueous wash impurity of low powered posterior chamber, then use the ethanol water eluting of the high number of degrees, get the Fructus Hippophae total flavones eluent;
(6) the gained eluent is condensed into cream, gets the Fructus Hippophae total flavones condensed cream;
(7) the Fructus Hippophae total flavones condensed cream is mixed silica gel, and the mixture that will mix through ethyl acetate and petroleum ether mixed liquor eluting, gets eluent as for the silicagel column top;
(8) eluent is reclaimed solvent after concentrate drying get the Fructus Hippophae total flavones semi-finished product;
(9) the Fructus Hippophae total flavones semi-finished product are dissolved with ethanol water, filter, Recycled ethanol, concentrated, place crystallize out, sucking filtration gets the Fructus Hippophae total flavones finished product.
In the described step (1), Fructus Hippophae carries out the ethanol water reflux, extract, after cleaning again, and the extraction solvent is 50%～85% ethanol water.
In the described step (1), the equipment that extracts is the countercurrent extraction production line, comprises elevator, charging transmission, countercurrent extraction tank group main frame 1, draws glassware 1, Juice squeezer 1, countercurrent extraction tank group main frame 2, draws glassware 2, Juice squeezer 2, discharging transmission, line pump, Pump for giving-out, temporary tank, heat exchanger, liquid flowing valve etc.Raw material is at the uniform velocity added by elevator charge door place behind the crushing screening, and extracting solution pumps via Pump for giving-out continuously from flowing to temporary storage tank.
In the described step (1), adverse current production line parameter is elevator frequency 15～30Hz, main frame 1 frequency 18～20Hz, Juice squeezer 1 frequency 45～50Hz, main frame 2 frequencies 20～22Hz, Juice squeezer 2 frequencies 40～45Hz, Pump for giving-out flow 0.5～2T/h, charging 100～400kg/h.
In the described step (4), the dilution water yield is 5 times of concentrated solution volume, filters to such an extent that impurity discards.
In the described step (5), the macroporous resin adsorption step adopts wet method dress post, keeps liquid level, and filtrate is passed through adsorption column, flow velocity per minute 0.05ml/g resin, and the resin model is HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous adsorbent resin.
In the described step (5), the macroporous adsorptive resins ratio of height to diameter is 10～5: 1, the ethanol water of low powered posterior chamber is 5%～20% ethanol water, the ethanol water of the high number of degrees is 50%～80% ethanol water, washing the impurity water yield is 3～5BV, the ethanol water amount of washing the impurity low powered posterior chamber is 1～2BV, and the ethanol water amount of the high number of degrees of eluting is 4BV.
In the described step (7), the silica gel column chromatography step adopts wet method dress post, keep liquid level, condensed cream is mixed the rear silica gel of activation by weight at 1: 1, and the mixture that will mix places the silicagel column top, eluent is ethyl acetate: the petroleum ether volume ratio is 50～85: 15 ethyl acetate and petroleum ether mixture, elution flow rate per minute 0.1ml/g silica gel, and elution volume is 5BV.The silica gel activating condition is 110 ℃ of 30min.
In the described step (9), the Fructus Hippophae total flavones semi-finished product are measured 60 ℃ of thermosols of 50% ethanol water with 12～16 times, and concentrated density is d=1.03～1.05.
The present invention discloses a kind of production new technique of Fructus Hippophae total flavones, the method is: drop into from cast hopper after raw material is cleaned, the rotation of extraction pot group main frame, material is slowly advanced backward from the unit front end, the feed tube that extracts simultaneously solvent slave group end enters in the extraction pot, pass mobile material forward end by the tank rear end and flow, the biphase material of solid-liquid is fully contact in this reverse movement, thereby with extracts active ingredients in the medical material out.Medicinal residues are forced to be pushed to slag notch and are discharged through the discharging conveyer, and special Juice squeezer pushes medicinal residues, and medicinal residues Shen residual liquor is extruded the medical material tissue, reduces medicinal residues Shen residual liquor content.Extraction efficiency is higher, extraction is more complete.
The present invention selects macroporous adsorbent resin and binding silica gel column chromatography purification simultaneously, and separating effect is better.
The specific embodiment:
Embodiment 1:
Take by weighing Fructus Hippophae 2T, at the uniform velocity added by the speed of elevator charge door with 400kg/h after cleaning, 75% ethanol water is added by feed tube with the flow of tubing pump with 2T/h, the elevator frequency setting is 30Hz, main frame 1 frequency setting is 20Hz, and Juice squeezer 1 frequency setting is 50Hz, and main frame 2 frequency settings are 22Hz, Juice squeezer 2 frequency settings are 45Hz, get Fructus Hippophae total flavones crude extract 10T; The Fructus Hippophae total flavones crude extract is concentrated to concentration tank via the Pump for giving-out continuous pump from flowing to temporary storage tank, gets the thick concentrated solution 600L of Fructus Hippophae total flavones; The gained concentrated solution is added the dilution of 3T water, remove by filter impurity; Filtrate is crossed the HPD400 macroporous adsorbent resin, and the resin column ratio of height to diameter is 5: 1, adsorbs saturated rear 6T washing impurity, 2T5% ethanol aqueous wash impurity, and 8T80% ethanol water eluting gets Fructus Hippophae total flavones eluent 7.8T; Eluent concentrates to get Fructus Hippophae total flavones condensed cream 400kg; The Fructus Hippophae total flavones condensed cream is mixed the 400kg activated silica gel, places the silicagel column top, and eluent is ethyl acetate: the petroleum ether volume ratio is 85: 15 ethyl acetate and petroleum ether mixture, and elution flow rate per minute 0.1ml/g silica gel gets eluent 2000kg; Concentrate drying got Fructus Hippophae total flavones semi-finished product 120kg after eluent reclaimed solvent; The Fructus Hippophae total flavones semi-finished product filter with 60 ℃ of thermosols of 1500L50% ethanol water, and Recycled ethanol is concentrated into d=1.05, place crystallize out, and sucking filtration gets Fructus Hippophae total flavones finished product 40kg, content 72%.
Embodiment 2:
Take by weighing Fructus Hippophae 800kg, at the uniform velocity added by the speed of elevator charge door with 200kg/h after cleaning, 65% ethanol water is added by feed tube with the flow of tubing pump with 1T/h, the elevator frequency setting is 25Hz, main frame 1 frequency setting is 18Hz, and Juice squeezer 1 frequency setting is 50Hz, and main frame 2 frequency settings are 22Hz, Juice squeezer 2 frequency settings are 45Hz, get Fructus Hippophae total flavones crude extract 4T; The Fructus Hippophae total flavones crude extract is concentrated to concentration tank via the Pump for giving-out continuous pump from flowing to temporary storage tank, gets the thick concentrated solution 250L of Fructus Hippophae total flavones; The gained concentrated solution is added the dilution of 1.25T water, remove by filter impurity; Filtrate is crossed the AB-8 macroporous adsorbent resin, and the resin column ratio of height to diameter is 5: 1, adsorbs saturated rear 6T washing impurity, 2T20% ethanol aqueous wash impurity, and 8T600% ethanol water eluting gets Fructus Hippophae total flavones eluent 7.8T; Eluent concentrates to get Fructus Hippophae total flavones condensed cream 150kg; The Fructus Hippophae total flavones condensed cream is mixed the 150kg activated silica gel, places the silicagel column top, and eluent is ethyl acetate: the petroleum ether volume ratio is 65: 15 ethyl acetate and petroleum ether mixture, and elution flow rate per minute 0.1ml/g silica gel gets eluent 750kg; Concentrate drying got Fructus Hippophae total flavones semi-finished product 50kg after eluent reclaimed solvent; The Fructus Hippophae total flavones semi-finished product filter with 60 ℃ of thermosols of 600L50% ethanol water, and Recycled ethanol is concentrated into d=1.04, place crystallize out, and sucking filtration gets Fructus Hippophae total flavones finished product 14kg, content 78%.
Embodiment 3:
Take by weighing Fructus Hippophae 1.6T, at the uniform velocity added by the speed of elevator charge door with 100kg/h after cleaning, 75% ethanol water is added by feed tube with the flow of tubing pump with 500kg/h, the elevator frequency setting is 25Hz, main frame 1 frequency setting is 18Hz, and Juice squeezer 1 frequency setting is 50Hz, and main frame 2 frequency settings are 22Hz, Juice squeezer 2 frequency settings are 45Hz, get Fructus Hippophae total flavones crude extract 8T; The Fructus Hippophae total flavones crude extract is concentrated to concentration tank via the Pump for giving-out continuous pump from flowing to temporary storage tank, gets the thick concentrated solution 500L of Fructus Hippophae total flavones; The gained concentrated solution is added the dilution of 2.5T water, remove by filter impurity; Filtrate is crossed the DM-130 macroporous adsorbent resin, and the resin column ratio of height to diameter is 5: 1, adsorbs saturated rear 6T washing impurity, 2T15% ethanol aqueous wash impurity, and 8T70% ethanol water eluting gets Fructus Hippophae total flavones eluent 7.8T; Eluent concentrates to get Fructus Hippophae total flavones condensed cream 310kg; The Fructus Hippophae total flavones condensed cream is mixed the 310kg activated silica gel, places the silicagel column top, and eluent is ethyl acetate: the petroleum ether volume ratio is 75: 15 ethyl acetate and petroleum ether mixture, and elution flow rate per minute 0.1ml/g silica gel gets eluent 15T; Concentrate drying got Fructus Hippophae total flavones semi-finished product 110kg after eluent reclaimed solvent; The Fructus Hippophae total flavones semi-finished product filter with 60 ℃ of thermosols of 1.6T50% ethanol water, and Recycled ethanol is concentrated into d=1.03, place crystallize out, and sucking filtration gets Fructus Hippophae total flavones finished product 28kg, content 74%.
Claims (9)
1. the production new technique of a Fructus Hippophae total flavones is characterized in that the method comprises the steps:
(1) Fructus Hippophae is cleaned the rear continuous countercurrent extracting tank ethanol water reflux, extract, that adds;
(2) extracting liquid filtering that will process through (1) gets the Fructus Hippophae total flavones crude extract;
(3) gained Fructus Hippophae total flavones crude extract is concentrated, get the thick concentrated solution of Fructus Hippophae total flavones;
(4) with the thick concentrated solution thin up of gained Fructus Hippophae total flavones, and filter, get filtrate;
(5) with the upper broad spectrum type macroporous resin adsorption post of gained filtrate, adsorb the complete impurity that washes with water, use again the ethanol aqueous wash impurity of low powered posterior chamber, then use the ethanol water eluting of the high number of degrees, get the Fructus Hippophae total flavones eluent;
(6) the gained eluent is condensed into cream, gets the Fructus Hippophae total flavones condensed cream;
(7) the Fructus Hippophae total flavones condensed cream is mixed silica gel, and the mixture that will mix through ethyl acetate with at oily ether mixed liquor eluting, gets eluent as for the silicagel column top;
(8) eluent is reclaimed solvent after concentrate drying get the Fructus Hippophae total flavones semi-finished product.
(9) the Fructus Hippophae total flavones semi-finished product are dissolved with ethanol water, filter, Recycled ethanol, concentrated, place crystallize out, sucking filtration gets the Fructus Hippophae total flavones finished product.
2. the production new technique of Fructus Hippophae total flavones according to claim 1 is characterized in that in the described step (1), and Fructus Hippophae carries out the ethanol water reflux, extract, after cleaning again, and the extraction solvent is 50%～85% ethanol water.
3. the production new technique of Fructus Hippophae total flavones according to claim 1 is characterized in that in the described step (1), the equipment that extracts is the countercurrent extraction production line, comprises elevator, charging transmission, countercurrent extraction tank group main frame 1, draws glassware 1, Juice squeezer 1, countercurrent extraction tank group main frame 2, draws glassware 2, Juice squeezer 2, discharging transmission, line pump, Pump for giving-out, temporary tank, heat exchanger, liquid flowing valve etc.Raw material is at the uniform velocity added by elevator charge door place behind the crushing screening, and extracting solution pumps via Pump for giving-out continuously from flowing to temporary storage tank.
4. the production new technique of Fructus Hippophae total flavones according to claim 1 is characterized in that in the described step (1), adverse current production line parameter is, elevator frequency 15～30Hz, main frame 1 frequency 18～20Hz, Juice squeezer 1 frequency 45～50Hz, main frame 2 frequencies 20～22Hz, Juice squeezer 2 frequencies 40～45Hz, Pump for giving-out flow 0.5～2T/h, charging 100～400kg/h.
5. the production new technique of Fructus Hippophae total flavones according to claim 1 is characterized in that in the described step (4), and the dilution water yield is 5 times of concentrated solution volume, filters to such an extent that impurity discards.
6. the production new technique of Fructus Hippophae total flavones according to claim 1 is characterized in that in the described step (5), the macroporous resin adsorption step adopts wet method dress post, keep liquid level, filtrate is passed through adsorption column, flow velocity per minute 0.05mll/g resin, resin model are HPD400, HPD100, DM-130 or AB-8 broad spectrum type macroporous adsorbent resin.
7. the production new technique of Fructus Hippophae total flavones according to claim 1 is characterized in that in the described step (5), the macroporous adsorptive resins ratio of height to diameter is 10～5: 1, the ethanol water of low powered posterior chamber is 5%～20% ethanol water, the ethanol water of the high number of degrees is 50%～80% ethanol water, washing the impurity water yield is 3～5BV, the ethanol water amount of washing the impurity low powered posterior chamber is 1～2BV, and the ethanol water amount of the high number of degrees of eluting is 4BV.
8. the production new technique of Fructus Hippophae total flavones according to claim 1 is characterized in that in the described step (7), the silica gel column chromatography step adopts wet method dress post, keep liquid level, condensed cream is mixed the rear silica gel of activation by weight at 1: 1, and the mixture that will mix places the silicagel column top, eluent is ethyl acetate: the petroleum ether volume ratio is 50～85: 15 ethyl acetate and petroleum ether mixture, elution flow rate per minute 0.1ml/g silica gel, and elution volume is 5BV.The silica gel activating condition is 110 ℃ of 30min.
9. the production new technique of Fructus Hippophae total flavones according to claim 1 is characterized in that in the described step (9), and the Fructus Hippophae total flavones semi-finished product are measured 60 ℃ of thermosols of 50% ethanol water with 12～16 times, and concentrated density is d=1.03～1.05.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103417588A (en) * | 2013-08-23 | 2013-12-04 | 中国科学院新疆理化技术研究所 | Preparation method of effective part of Hippophae rhamnoides |
| CN103690693A (en) * | 2013-12-13 | 2014-04-02 | 大兴安岭嘉迪欧营养原料有限公司 | Novel preparation technology of violet general flavone |
| CN104127356A (en) * | 2014-08-07 | 2014-11-05 | 中国科学院新疆理化技术研究所 | Sea-buckthorn oropharynx antibacterial and antiphlogistic compositional liquid and preparation method thereof |
| CN107281234A (en) * | 2016-06-13 | 2017-10-24 | 中国科学院西北高原生物研究所 | A kind of Hippophate flavone class extract and preparation method thereof |
| CN108244649A (en) * | 2018-03-20 | 2018-07-06 | 湖南中沙中医科技有限公司 | There is hippophae rhamnoides fruit oil soft capsule for softening blood vessel and preparation method thereof |
| CN110548053A (en) * | 2018-06-04 | 2019-12-10 | 大兴安岭至臻尚品寒带生物技术有限公司 | a method for preparing fructus Hippophae extract rich in total flavonoids and natural vitamin C |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103417588A (en) * | 2013-08-23 | 2013-12-04 | 中国科学院新疆理化技术研究所 | Preparation method of effective part of Hippophae rhamnoides |
| CN103690693A (en) * | 2013-12-13 | 2014-04-02 | 大兴安岭嘉迪欧营养原料有限公司 | Novel preparation technology of violet general flavone |
| CN104127356A (en) * | 2014-08-07 | 2014-11-05 | 中国科学院新疆理化技术研究所 | Sea-buckthorn oropharynx antibacterial and antiphlogistic compositional liquid and preparation method thereof |
| CN107281234A (en) * | 2016-06-13 | 2017-10-24 | 中国科学院西北高原生物研究所 | A kind of Hippophate flavone class extract and preparation method thereof |
| CN108244649A (en) * | 2018-03-20 | 2018-07-06 | 湖南中沙中医科技有限公司 | There is hippophae rhamnoides fruit oil soft capsule for softening blood vessel and preparation method thereof |
| CN110548053A (en) * | 2018-06-04 | 2019-12-10 | 大兴安岭至臻尚品寒带生物技术有限公司 | a method for preparing fructus Hippophae extract rich in total flavonoids and natural vitamin C |
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Free format text: CORRECT: APPLICANT; FROM: GREAT XINGAN MOUNTAINS LINGEBEI ORGANIC FOOD CO., LTD. TO: GREATER KHINGAN MOUNTAIN LINGONBERRY BIOTECHNOLOGY CO., LTD. |
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| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20130424 |
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| RJ01 | Rejection of invention patent application after publication |