CN102058712A - Rehmannia stem and leaf extract and preparation method and application thereof - Google Patents

Rehmannia stem and leaf extract and preparation method and application thereof Download PDF

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Publication number
CN102058712A
CN102058712A CN2009102017985A CN200910201798A CN102058712A CN 102058712 A CN102058712 A CN 102058712A CN 2009102017985 A CN2009102017985 A CN 2009102017985A CN 200910201798 A CN200910201798 A CN 200910201798A CN 102058712 A CN102058712 A CN 102058712A
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stem
rehmannic
glutinous
leaf extract
ethanol
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玄振玉
黄孝春
陆琪
吴惠
吴立怀
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SHANGHAI YOUSEEN NEW MEDICINE EXPLOITATION CO Ltd
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SHANGHAI YOUSEEN NEW MEDICINE EXPLOITATION CO Ltd
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Abstract

The invention belongs to the technical field of medicines, and in particular relates to a rehmannia stem and leaf extract, which is prepared by the following steps of: (1) crushing rehmannia stem and leaf, and heating by using water for reflux extraction to obtain extracting solution; (2) filtering the extracting solution, and concentrating filtrate to obtain concentrated solution A; (3) adding ethanol into the concentrated solution A, standing overnight, taking the filtrate, and obtaining ethanol precipitation solution B; (4) recovering the ethanol from the ethanol precipitation solution B, and concentrating to obtain concentrated solution C; (5) applying the concentrated solution C to macroporous adsorbent resin, eluting with water, discarding eluent, eluting with ethanol, collecting eluent, recovering the ethanol, and concentrating to obtain extractum D; and (6) drying the extractum D. The rehmannia stem and leaf extract is characterized in that the catalpol content is over 50 percent. The invention also provides application of the rehmannia stem and leaf extract in preparing medicines or health care products for improving neurological deficits following focal cerebral ischemia, and reducing blood sugar.

Description

A kind of glutinous rehmannic stem and leaf extract and its production and use
Technical field
The present invention relates to a kind of glutinous rehmannic stem and leaf extract; In addition, the invention still further relates to this glutinous rehmannic stem and leaf preparation method of extract and purposes.
Background technology
Ginseng section herbaceos perennial generally is fresh or dried root is used as medicine.Modern scientific research shows that Radix Rehmanniae contains number of chemical compositions such as iridoid glycosides, monoterpene and glycoside thereof, oligosaccharides, amino acids.Catalpol is the iridoid monoglycosides that content is the highest in the Radix Rehmanniae, is one of main active of Radix Rehmanniae, has blood sugar lowering and the effect of protection cranial nerve.The glutinous rehmannic stem and leaf routine is considered to there is not medical value, and active constituent content is little can not be counted, and generally also not as medical material, and disposes as garbage.Utilize herb resource in order to save, present patent application inventor has carried out research in depth to glutinous rehmannic stem and leaf, finds that the extract of glutinous rehmannic stem and leaf can be used as raw material, is used to prepare the medicine or the health product of blood sugar lowering and protection cranial nerve.
Find that through patent retrieval the patent that relates to the glutinous rehmannic stem and leaf extract has 1 piece, application number is: CN200410062245.3, patent name: the extraction process of glutinous rehmannic stem and leaf total heteroside extract.This patent disclosure the preparation method of glutinous rehmannic stem and leaf total heteroside, the technical characterictic of its preparation method is by the active carbon detached dowel, with the organic solvent eluting of low concentration.Claim that according to this patent specification this preparation method obtains the iridoid glycoside constituents more than 50%, catalpol content is greater than 20%.
The characteristics of cyclic terpenoid compounds such as catalpol are structure proximates, poor stability, and polarity is very big, is soluble in high polar solvent.The inventor finds that through the experiment sieving of system there is flaw in the preparation technology of above-mentioned CN200410062245.3 patent, mainly shows: it is improper that (1) adopts active carbon to do adsorbent.Active carbon is a kind of good adsorbent, and it has the double grading of physical absorption and chemisorbed, can selectively adsorb the various materials in gas phase, the liquid phase, to reach purposes such as decolorizing and refining, disinfecting, deodorizing and decontamination purification.Active carbon has the crystallite that image-stone smoky quartz grain is but irregularly arranged, and active carbon is a nonpolar molecule, is easy to adsorb adsorbate nonpolar or that polarity is very low.And the iridoid glycosides in the glutinous rehmannic stem and leaf mostly is the strong polar component of water solublity, and therefore selecting active carbon is inappropriate as the separating filler of glutinous rehmannic stem and leaf total heteroside.(2) absorption back eluting is relatively more difficult.Publication adopts washing, be lower than 10% ethanol aqueous wash, be higher than ethanol aqueous wash more than 10% or the like.Lengthy complexity on technology, the wasting of resources is many.(3) eluent select for use and consumption unreasonable.In the technical scheme that publication provides, one of its essential features promptly adopts the conventional flush away impurity of water to colourless, or further adopts and be lower than 10% ethanol, be lower than 15% methanol or be lower than 10% acetone soln that to be washed till eluent colourless.Consumption to eluant is not done qualification, and can cause a large amount of is that the iridoid glycoside constituents of representative runs off from activated-charcoal column with the catalpol, causes serious waste, has also finally caused the content of catalpol in its finished product lower.
The inventor of present patent application is through a large amount of tests, determined a kind of method that from glutinous rehmannic stem and leaf, prepares the glutinous rehmannic stem and leaf extract, and according to this method, prepared a kind of new glutinous rehmannic stem and leaf extract, catalpol content is significantly higher than the glutinous rehmannic stem and leaf total heteroside that publication prepares in this extract.The inventor herein has also explored preparation method of extract and application pharmaceutically simultaneously.
Summary of the invention
At the deficiencies in the prior art, the purpose of this invention is to provide a kind of glutinous rehmannic stem and leaf extract; Another object of the present invention provides this glutinous rehmannic stem and leaf preparation method of extract and purposes.
A kind of glutinous rehmannic stem and leaf extract provided by the invention is that the aerial parts from Radix Rehmanniae is to extract the stem and leaf, wherein contains catalpol more than 50%.
Glutinous rehmannic stem and leaf extract provided by the invention can combine with pharmaceutic adjuvant, makes clinical acceptable various pharmaceutical preparatioies.
Glutinous rehmannic stem and leaf extract of the present invention prepares by the following method:
(1) with after the glutinous rehmannic stem and leaf pulverizing, the water heating and refluxing extraction gets extracting solution;
(2) with extracting liquid filtering, filtrate concentrates, and gets concentrated solution A;
(3) concentrated solution A is added ethanol, placement is spent the night, and gets filtrate, gets alcohol deposit fluid B;
(4) alcohol deposit fluid B is reclaimed ethanol, concentrated, get concentrated solution C;
(5) concentrated solution C is gone up macroporous adsorbent resin, water elution discards eluent, with ethanol elution, collects eluent, reclaims ethanol, and concentrating under reduced pressure gets extractum D;
(6) with extractum D drying, promptly.
Preferably, glutinous rehmannic stem and leaf extract of the present invention prepares by the following method:
(1) with after the glutinous rehmannic stem and leaf pulverizing, the water heating and refluxing extraction gets extracting solution;
(2) with extracting liquid filtering, filtrate is concentrated into relative density 1.08-1.15 (50 ℃), gets concentrated solution A;
(3) concentrated solution A is added 95% ethanol to determining alcohol 60-80%, placement is spent the night, and gets filtrate, gets alcohol deposit fluid B;
(4) alcohol deposit fluid B is reclaimed ethanol, is concentrated into relative density 1.05-1.1 (50 ℃), get concentrated solution C;
(5) concentrated solution C is gone up macroporous adsorbent resin,, discard eluent, doubly measure the ethanol elution that concentration is 5-10%, collect eluent, reclaim ethanol, be concentrated into relative density 1.1-1.3 (50 ℃), get extractum D with column volume 1-5 with 1~5 times of water gaging eluting;
(6), pulverize, promptly with extractum D drying.
In above-mentioned steps (5), described macroporous adsorbent resin adopts XAD-1600, XAD-16, PRP-2A, a kind of among the PRP-5A.
Glutinous rehmannic stem and leaf extract provided by the invention function of nervous system after the preparation cerebral ischemia improves the application in medicine or the health product.
The application of glutinous rehmannic stem and leaf extract provided by the invention in preparation hypoglycemic drug or health product.
Advantage of the present invention: catalpol content is more than 50% in the resulting final products of a kind of glutinous rehmannic stem and leaf extract of the present invention; can guarantee good blood sugar lowering and the effect of protection cranial nerve; based on the total iridoid glycoside, it is about 20% good that catalpol only accounts for than patent CN200410062245.3.Adopt macroporous adsorptive resins to have the better effect of specific activity charcoal adsorption column in the preparation method of the present invention, and technology is simple, does not use toxic solvent, industrial pollution is little, and cost is low.
Description of drawings
Fig. 1. the evaluation figure of catalpol content more than 50%
Fig. 2. catalpol standard substance figure
Pharmacodynamic experiment (one)
1 experiment purpose: investigate the drug action that glutinous rehmannic stem and leaf extract of the present invention improves nervous function behind the rat cerebral ischemia in vivo.
2 experiment materials:
2.1 tested medicine: glutinous rehmannic stem and leaf extract (according to the medicine of the present invention of embodiment 4 preparations), with physiological saline solution (matching while using).
2.2 animal used as test: the SD rat, male, body weight 270~300g is provided by Test Animal Centre, Academy of Military Medical Sciences, P.L.A, credit number: SCXK (army) 2007-0004.
3 experimental techniques
Get 40 of rats, establish sham-operation group, model group, glutinous rehmannic stem and leaf extract 60,20mg/kg group. After the modeling 3 days, according to behavioral experiment scoring random packet, 10 every group, and the beginning administration.
The rat cerebral ischemia model method: rat is anaesthetized with 10% chloraldurate 350mg/kg, and back of the body position is fixing, separates right carotid, peels off external carotid artery, internal carotid; Ligation arteria carotis communis, external carotid artery, the artery clamp folder closes internal carotid. Insert fishing line (diameter 0.25mm) in arteria carotis communis, open artery clamp, bolt enters fishing line (being deep to 18mm), fixedly fishing line. Sew up a wound to steam again and raise.
Medication: glutinous rehmannic stem and leaf extract 60mg/kg group: glutinous rehmannic stem and leaf extract 240mg is molten to the 4ml gastric infusion, and the administration volume is 0.1ml/100g body weight, i.e. 60mg/kg; Glutinous rehmannic stem and leaf extract 20mg/kg group: glutinous rehmannic stem and leaf extract 80mg is molten to the 4ml gastric infusion, and the administration volume is 0.1ml/100g body weight, i.e. 20mg/kg; Sham-operation group, model group gavage every day give equivalent drinking water 0.1ml/100g body weight.
Index determining: the strong rear flank limb tenderness pain threshold that after administration, carried out respectively the bilateral forelimb grip of behavior scoring, beam walking test, mensuration rat, strong side forelimb perceptibility and mensuration rat on the the 3rd, 6,9 day.
Behavior scoring:
(1) carries the about chi of mouse tail built on stilts, observe forelimb flexing situation. Stretch to ground such as two forelimb symmetries, be designated as 0 fen; As the flexing that shoulder flexing, elbow flexing, shoulder inward turning or existing wrist elbow appear in the offside forelimb of performing the operation has again inward turning person, is designated as 1 fen.
(2) animal is placed on the level and smooth ground, push away respectively both shoulders to side shifting, check resistance. Be designated as 0 fen such as bilateral resistance equity and strong person; The resistance descender is designated as 1 fen when promoting to the operation offside.
(3) animal two forelimbs are put on the wire netting, observed the flesh tension force of two forelimbs. Bilateral flesh tension force equity and strong person are 0 minute; Operation offside muscle of anterior limb tension force descends and is designated as 1 fen.
(4) carry the about chi of mouse tail built on stilts, animal has ceaselessly to operation offside revolver, is designated as 1 fen; Otherwise, be designated as 0 fen. According to above standard scoring, full marks are 4 minutes, and mark is more high, and the behavior disorder of animal is more serious.
Beam walking experiment: the coordination of beam walking experimental evaluation campaign and integrate damaged. The wide 2.0cm of beam, long 120cm, thick 1cm,, apart from the unsettled placement of ground 80cm level, beam one end connects a magazine (long 25cm, wide 22cm, high 18cm), comes into magazine with the noise stimulation rat by beam. Standards of grading: rat can not stay on the beam, 0 minute; Rat can stay on the beam but be motionless, 1 minute; Rat attempt by, but throw 2 fens from beam; Rat walks upper cord, but the hind leg landing number of times of damage was above 50%, 3 minute; Above 1 time but less than 50%, 4 minute; Only landing is 1 time, 5 minutes; Pass through smoothly 6 fens. Training is 2 days before the ischemic, allows rat learn to pass by smoothly beam. To detect respectively for observing time point in 3,6,9 days behind the ischemic.
Haptic stimulus experiment: estimate somatesthesia and fine movement and carry out function. Medical proof fabric with equal area (0.7cm*0.7cm) is attached to rat left fore wrist facies ventralis as haptic stimulus, and the record rat removes the incubation period of adhesive plaster. Preoperative exercise 2 days, makes rat can finish the action that removes adhesive plaster in 20 seconds by 1 times/day. To detect respectively for observing time point in 3,6,9 days behind the ischemic.
The bilateral forelimb grip test of rat: animal grip tester test.
The strong rear flank limb tenderness pain threshold test of rat: animal tenderness tester test.
4 experimental results
Between various detected values are organized relatively, the t check. The results are shown in Table.
Table 1.1 glutinous rehmannic stem and leaf extract of the present invention is to the impact of cerebral ischemia subacute stage rat nervous symptoms scoring
Annotate: compare with model group *P<0.05, *P<0.01
Table 1.2 glutinous rehmannic stem and leaf extract of the present invention is to the influence of the strong side forelimb grip of cerebral ischemia subacute stage rat
Figure B2009102017985D0000052
Annotate: compare with model group *P<0.05, *P<0.01
Table 1.3 glutinous rehmannic stem and leaf extract of the present invention is to the influence of the refreshing strong rear flank of cerebral ischemia subacute stage rat limb tenderness pain threshold
Figure B2009102017985D0000053
Annotate: compare with model group *P<0.05, *P<0.01
Table 1.4 glutinous rehmannic stem and leaf extract of the present invention is to the influence of cerebral ischemia subacute stage rat beam walking experiment scoring
Annotate: compare with model group *P<0.05, *P<0.01
Table 1.5 glutinous rehmannic stem and leaf extract of the present invention is to the strong tactile influence of side forelimb of cerebral ischemia subacute stage rat
Figure B2009102017985D0000055
Annotate: compare with model group *P<0.05, *P<0.01
5 experiment conclusion
This research adopts suture method to prepare the rat cerebral ischemia model, and orally give medicine of the present invention after 3 days was observed after the administration improvement of rat function of nervous system 3-9 days.Experimental observation 5 indexs, the result shows, medicine 60 of the present invention, 20mg/kg group all have certain function of nervous system's effect after the cerebral ischemia that improves, medicine 60mg/kg group wherein of the present invention has superiority slightly, there were significant differences for four indices.
Pharmacodynamic experiment (two)
1 experiment purpose
The hypoglycemic activity of zoopery checking glutinous rehmannic stem and leaf extract of the present invention
2 experiment materials
2.1 laboratory animal: SPF level, 50 of spontaneous obese diabetic mices (db/db mice), age in 5-6 week, body weight 38 ± 2g, random packet.Provide by Chinese Academy of Sciences zoopery center.
2.2 experiment medicine: glutinous rehmannic stem and leaf extract 60mg/kg of the present invention, glutinous rehmannic stem and leaf extract 20mg/kg of the present invention; Positive control drug is rosiglitazone maleate (a GlaxoSmithKline PLC Tianjin pharmaceutcal corporation, Ltd), one touchII blood glucose meter (Johson ﹠ Johnson).
3 experimental techniques
3.1 animal grouping
Model control group: 10.Give and wait water gaging.
Positive controls: 10.Give positive drug.
Experiment medicine group: 20, being divided into is two groups, gives glutinous rehmannic stem and leaf extract 60mg/kg of the present invention, glutinous rehmannic stem and leaf extract 20mg/kg of the present invention respectively.
3.2 administration
The grouping back adapts to week beginning administration, and in 2 weeks of successive administration, route of administration is for irritating stomach.
Glutinous rehmannic stem and leaf extract 60mg/kg group: glutinous rehmannic stem and leaf extract 240mg is molten to the 4ml gastric infusion, and the administration volume is 0.1ml/100g body weight, i.e. 60mg/kg; Glutinous rehmannic stem and leaf extract 20mg/kg group: glutinous rehmannic stem and leaf extract 80mg is molten to the 4ml gastric infusion, and the administration volume is 0.1ml/100g body weight, i.e. 20mg/kg; Model group is irritated stomach and give equivalent drinking water 0.1ml/100g body weight every day; The positive controls rosiglitazone maleate is irritated stomach 3mg/kg every day.
3.3 blood sugar detection
3rd, administration in 6,9 days is after 1 hour, and the tail vein is got blood and measured animal blood glucose immediately with one touch II blood glucose meter.
4 experimental results
Table 2.1 glutinous rehmannic stem and leaf extract of the present invention to the influence of db/db mouse blood sugar concentration (x ± s, mM)
Figure B2009102017985D0000071
Table 2.1 shows, that positive controls mouse blood sugar concentration reaches is minimum (the t check, *P<0.05vs model group), the results suggest experimental animal model is reliable.Glutinous rehmannic stem and leaf extract treated animal blood sugar concentration of the present invention than model group all have significant reduction (t check, *P<0.05vs model group, *P<0.01vs model group), glutinous rehmannic stem and leaf extract 20mg/kg wherein of the present invention, 60mg/kg group all has hypoglycemic activity, and wherein the 60mg/kg group is more excellent.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.These embodiment are interpreted as only being used to the present invention is described and are not used in restriction protection scope of the present invention.After the content of having read the present invention's record, those skilled in the art can make various changes or modifications the present invention, and these equivalences change and modify and fall into claim of the present invention institute restricted portion equally.
Embodiment 1
After the glutinous rehmannic stem and leaf pulverizing, get 50kg, add 600L water heating and refluxing extraction twice, each 1h, merge extractive liquid.With extracting liquid filtering, get filtrate and be concentrated into relative density 1.11 (50 ℃) at 70 ℃, get concentrated solution A; Concentrated solution A is added 95% ethanol to determining alcohol reach 60%, placement is spent the night, and filters, and gets filtrate and gets alcohol deposit fluid B; Alcohol deposit fluid B is reclaimed ethanol at 70 ℃, be concentrated into the concentrated solution C of relative density 1.09 (50 ℃).Concentrated solution C is gone up the PRP-2A macroporous adsorptive resins, wash resin column, discard water liquid with 2.5 times of water gagings of resin column volume, 10% ethanol elution of 3 times of amounts of reuse resin column volume, collect ethanol elution, reclaim ethanol and be evaporated to relative density 1.28 (50 ℃), get extractum.With extractum vacuum decompression drying, pulverizing must be yellow to brown ceramic powder shape glutinous rehmannic stem and leaf extract 1.44kg, records to contain catalpol 67%.
Embodiment 2
After the glutinous rehmannic stem and leaf pulverizing, get 50kg, add 600L water heating and refluxing extraction twice, each 1h, merge extractive liquid.With extracting liquid filtering, get filtrate and be concentrated into relative density 1.09 (50 ℃) at 80 ℃, get concentrated solution A; Concentrated solution A is added 95% ethanol to determining alcohol reach 70%, placement is spent the night, and filters, and gets filtrate and gets alcohol deposit fluid B; Alcohol deposit fluid B is reclaimed ethanol at 70 ℃, be concentrated into the concentrated solution C of relative density 1.08 (50 ℃).Concentrated solution C is gone up the XAD-1600 macroporous adsorptive resins, wash resin column, discard water liquid with 1 times of water gaging of resin column volume, 5% ethanol elution of 2 times of amounts of reuse resin column volume, collect ethanol elution, reclaim ethanol and be evaporated to relative density 1.20 (50 ℃), get extractum.With extractum vacuum decompression drying, pulverizing must be yellow to brown ceramic powder shape glutinous rehmannic stem and leaf extract 1.48kg, records to contain catalpol 58%.
Embodiment 3
After the glutinous rehmannic stem and leaf pulverizing, get 50kg, add 500L water heating and refluxing extraction three times, each 1h, merge extractive liquid.With extracting liquid filtering, get filtrate and be concentrated into relative density 1.14 (50 ℃) at 80 ℃, get concentrated solution A; Concentrated solution A is added 95% ethanol to determining alcohol reach 80%, placement is spent the night, and filters, and gets filtrate and gets alcohol deposit fluid B; Alcohol deposit fluid B is reclaimed ethanol at 70 ℃, be concentrated into the concentrated solution C of relative density 1.06 (50 ℃).Concentrated solution C is gone up the XAD-1600 macroporous adsorptive resins, wash resin column, discard water liquid with 1.5 times of water gagings of resin column volume, 10% ethanol elution of 3 times of amounts of reuse resin column volume, collect ethanol elution, reclaim ethanol and be evaporated to relative density 1.3 (50 ℃), get extractum.With extractum vacuum decompression drying, pulverizing must be yellow to brown ceramic powder shape glutinous rehmannic stem and leaf extract 1.51kg, records to contain catalpol 55%.
Embodiment 4
After the glutinous rehmannic stem and leaf pulverizing, get 50kg, add 500L water heating and refluxing extraction three times, each 1h, merge extractive liquid.With extracting liquid filtering, get filtrate and be concentrated into relative density 1.12 (50 ℃) at 70 ℃, get concentrated solution A; Concentrated solution A is added 95% ethanol to determining alcohol reach 70%, placement is spent the night, and filters, and gets filtrate, gets alcohol deposit fluid B; Alcohol deposit fluid B is reclaimed ethanol at 70 ℃, be concentrated into the concentrated solution C of relative density 1.08 (50 ℃).Concentrated solution C is gone up the XAD-16 macroporous adsorptive resins, wash resin column, discard water liquid with 3 times of water gagings of resin column volume, 5% ethanol elution of 3 times of amounts of reuse resin column volume, collect ethanol elution, reclaim ethanol and be evaporated to relative density 1.20 (50 ℃), get extractum.With extractum vacuum decompression drying, pulverizing must be yellow to brown ceramic powder shape glutinous rehmannic stem and leaf extract 1.56kg, records to contain catalpol 56%.
Embodiment 5
After the glutinous rehmannic stem and leaf pulverizing, get 50kg, add 500L water heating and refluxing extraction three times, each 1h, merge extractive liquid.With extracting liquid filtering, get filtrate and be concentrated into relative density 1.08 (50 ℃) at 70 ℃, get concentrated solution A; Concentrated solution A is added 95% ethanol to determining alcohol reach 70%, placement is spent the night, and filters, and gets filtrate, gets alcohol deposit fluid B; Alcohol deposit fluid B is reclaimed ethanol at 70 ℃, be concentrated into the concentrated solution C of relative density 1.05 (50 ℃).Concentrated solution C is gone up the PRP-5A macroporous adsorptive resins, wash resin column, discard water liquid with 5 times of water gagings of resin column volume, 10% ethanol elution of 3 times of amounts of reuse resin column volume, collect ethanol elution, reclaim ethanol and be evaporated to relative density 1.1 (50 ℃), get extractum.With extractum vacuum decompression drying, pulverizing must be yellow to brown ceramic powder shape glutinous rehmannic stem and leaf extract 1.42kg, records to contain catalpol 59%.
Embodiment 6
After the glutinous rehmannic stem and leaf pulverizing, get 50kg, add 500L water heating and refluxing extraction three times, each 1h, merge extractive liquid.With extracting liquid filtering, get filtrate and be concentrated into relative density 1.15 (50 ℃) at 70 ℃, get concentrated solution A; Concentrated solution A is added 95% ethanol to determining alcohol reach 80%, placement is spent the night, and filters, and gets filtrate, gets alcohol deposit fluid B; Alcohol deposit fluid B is reclaimed ethanol at 70 ℃, be concentrated into the concentrated solution C of relative density 1.1 (50 ℃).Concentrated solution C is gone up the PRP-5A macroporous adsorptive resins, wash resin column, discard water liquid with 3 times of water gagings of resin column volume, 5% ethanol elution of 5 times of amounts of reuse resin column volume, collect ethanol elution, reclaim ethanol and be evaporated to relative density 1.3 (50 ℃), get extractum.With extractum vacuum decompression drying, pulverizing must be yellow to brown ceramic powder shape glutinous rehmannic stem and leaf extract 1.45kg, records to contain catalpol 61%.

Claims (7)

1. glutinous rehmannic stem and leaf extract is characterized in that this glutinous rehmannic stem and leaf extract prepares by the following method:
(1) with after the glutinous rehmannic stem and leaf pulverizing, the water heating and refluxing extraction gets extracting solution;
(2) with extracting liquid filtering, filtrate concentrates, and gets concentrated solution A;
(3) concentrated solution A is added ethanol, placement is spent the night, and gets filtrate, gets alcohol deposit fluid B;
(4) alcohol deposit fluid B is reclaimed ethanol, concentrated, get concentrated solution C;
(5) concentrated solution C is gone up macroporous adsorbent resin, water elution discards eluent, with ethanol elution, collects eluent, reclaims ethanol, concentrates, and gets extractum D;
(6) with extractum D drying, promptly get the glutinous rehmannic stem and leaf extract.
2. a kind of glutinous rehmannic stem and leaf extract according to claim 1 is characterized in that preparing by the following method:
(1) with after the glutinous rehmannic stem and leaf pulverizing, the water heating and refluxing extraction gets extracting solution;
(2) with extracting liquid filtering, filtrate is concentrated into 50 ℃ of relative density 1.08-1.15, gets concentrated solution A;
(3) concentrated solution A is added 95% ethanol to determining alcohol 60-80%, placement is spent the night, and gets filtrate, gets alcohol deposit fluid B;
(4) alcohol deposit fluid B is reclaimed ethanol, is concentrated into 50 ℃ of relative density 1.05-1.1, get concentrated solution C;
(5) concentrated solution C is gone up macroporous adsorbent resin,, discard eluent, doubly measure the ethanol elution that concentration is 5-10%, collect eluent, reclaim ethanol, be concentrated into 50 ℃ of relative density 1.1-1.3, get extractum D with column volume 1-5 with 1~5 times of water gaging eluting;
(6) with extractum D drying, pulverize, promptly get the glutinous rehmannic stem and leaf extract.
3. a kind of glutinous rehmannic stem and leaf extract according to claim 1 and 2 is characterized in that catalpol content is more than 50%.
4. a kind of glutinous rehmannic stem and leaf extract according to claim 1 and 2 is characterized in that (5) step of described preparation method macroporous adsorbent resin adopts a kind of among XAD-1600, XAD-16, PRP-2A, the PRP-5A.
5. the application of glutinous rehmannic stem and leaf extract according to claim 1 and 2 is characterized in that preparing medicine or pharmaceutical composition with at least a pharmaceutically acceptable inert matter.
6. glutinous rehmannic stem and leaf extract provided by the invention medicine that function of nervous system improves after the preparation cerebral ischemia or the application in the health product.
7. the application of glutinous rehmannic stem and leaf extract provided by the invention in preparation hypoglycemic drug or health product.
CN2009102017985A 2009-11-13 2009-11-13 Rehmannia stem and leaf extract and preparation method and application thereof Pending CN102058712A (en)

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CN102863489A (en) * 2011-07-04 2013-01-09 苏州玉森新药开发有限公司 Method for extracting catalpol from rehmannia stem
CN102885244A (en) * 2011-07-21 2013-01-23 苏州玉森新药开发有限公司 New application of catalpol in health-care product and food
CN102885314A (en) * 2011-07-20 2013-01-23 苏州玉森新药开发有限公司 Novel use of catalpol in health products and foods taken by people suffering from cerebral arterial thrombosis reperfusion injuries
CN103054895A (en) * 2013-01-16 2013-04-24 济南康众医药科技开发有限公司 Medicine composition for preventing and treating obesity
CN104382980A (en) * 2014-11-14 2015-03-04 中国科学院西双版纳热带植物园 Plukenetia volubilis L. stem leaf extract capable of delaying senescence as well as preparation method and application of extract
CN106220695A (en) * 2016-07-21 2016-12-14 西安岳达生物科技股份有限公司 A kind of industrial production process of catalpol
CN108059646A (en) * 2017-12-27 2018-05-22 扬州工业职业技术学院 The preparation method of hypoglycemic activity ingredient in a kind of radix rehmanniae recen
CN108084232A (en) * 2017-12-27 2018-05-29 扬州工业职业技术学院 A kind of glucokinase activators and its application in hypoglycemic medicine is prepared
CN112494379A (en) * 2020-11-18 2021-03-16 广州巴宝莉化妆品有限公司 Plant composition, preparation method and application in shampoo
CN113480581A (en) * 2021-07-21 2021-10-08 湖南朗林生物资源股份有限公司 Method for extracting iridoid glycoside from rehmannia

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03271227A (en) * 1990-03-20 1991-12-03 Tsumura & Co Therapeutic agent for treating diabetes mellitus
CN1715285A (en) * 2004-07-02 2006-01-04 罗何生 Process for extracting glutinous rehmannic stem and leaf total heteroside extract
CN1947757A (en) * 2006-09-16 2007-04-18 四川美大康药业股份有限公司 Leave of glutinous rehmannia extractive, its prepn. method and use, medicines prepd. with said extractives
CN101099789A (en) * 2007-07-18 2008-01-09 张玲 Hypoglycemic, antilipenic and treating hemopathy glutinous rehmannia extract and preparing method

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPH03271227A (en) * 1990-03-20 1991-12-03 Tsumura & Co Therapeutic agent for treating diabetes mellitus
CN1715285A (en) * 2004-07-02 2006-01-04 罗何生 Process for extracting glutinous rehmannic stem and leaf total heteroside extract
CN1947757A (en) * 2006-09-16 2007-04-18 四川美大康药业股份有限公司 Leave of glutinous rehmannia extractive, its prepn. method and use, medicines prepd. with said extractives
CN101099789A (en) * 2007-07-18 2008-01-09 张玲 Hypoglycemic, antilipenic and treating hemopathy glutinous rehmannia extract and preparing method

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102863489A (en) * 2011-07-04 2013-01-09 苏州玉森新药开发有限公司 Method for extracting catalpol from rehmannia stem
CN102885314A (en) * 2011-07-20 2013-01-23 苏州玉森新药开发有限公司 Novel use of catalpol in health products and foods taken by people suffering from cerebral arterial thrombosis reperfusion injuries
CN102885244A (en) * 2011-07-21 2013-01-23 苏州玉森新药开发有限公司 New application of catalpol in health-care product and food
CN103054895A (en) * 2013-01-16 2013-04-24 济南康众医药科技开发有限公司 Medicine composition for preventing and treating obesity
CN104382980B (en) * 2014-11-14 2018-08-17 中国科学院西双版纳热带植物园 It is a kind of that there is the astral oil rattan leaf extract to slow down aging and its preparation and application
CN104382980A (en) * 2014-11-14 2015-03-04 中国科学院西双版纳热带植物园 Plukenetia volubilis L. stem leaf extract capable of delaying senescence as well as preparation method and application of extract
CN106220695A (en) * 2016-07-21 2016-12-14 西安岳达生物科技股份有限公司 A kind of industrial production process of catalpol
CN108059646A (en) * 2017-12-27 2018-05-22 扬州工业职业技术学院 The preparation method of hypoglycemic activity ingredient in a kind of radix rehmanniae recen
CN108084232A (en) * 2017-12-27 2018-05-29 扬州工业职业技术学院 A kind of glucokinase activators and its application in hypoglycemic medicine is prepared
CN108084232B (en) * 2017-12-27 2019-10-01 扬州工业职业技术学院 A kind of glucokinase activators and its preparing the application in hypoglycemic medicine
CN112494379A (en) * 2020-11-18 2021-03-16 广州巴宝莉化妆品有限公司 Plant composition, preparation method and application in shampoo
CN112494379B (en) * 2020-11-18 2023-09-08 广州巴宝莉化妆品有限公司 Plant composition, preparation method and application thereof in shampoo
CN113480581A (en) * 2021-07-21 2021-10-08 湖南朗林生物资源股份有限公司 Method for extracting iridoid glycoside from rehmannia
CN113480581B (en) * 2021-07-21 2022-05-24 湖南朗林生物资源股份有限公司 Method for extracting iridoid glycoside from rehmannia

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