CN104142046A - Method for drying eucommia ulmoides - Google Patents
Method for drying eucommia ulmoides Download PDFInfo
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- CN104142046A CN104142046A CN201410418477.1A CN201410418477A CN104142046A CN 104142046 A CN104142046 A CN 104142046A CN 201410418477 A CN201410418477 A CN 201410418477A CN 104142046 A CN104142046 A CN 104142046A
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Abstract
The invention relates to a method for drying eucommia ulmoides. The method comprises the following steps: taking fresh eucommia ulmoides, stacking for transpiration until the under bark is purple brown, and performing freeze-drying until sublimation is ended. The prepared eucommia ulmoides is high in content of multiple active ingredients and good in clinical curative effect.
Description
Invention field
The present invention relates to medicine method for making, particularly a kind of drying means of the bark of eucommia, belongs to medical technical field.
Background technology
Traditional Chinese medicine drying has very long history in China, the Chinese herbal medicine of drying can keep certain medicinal ingredient and be difficult for putrid and deteriorated, the dry important measures as guaranteeing Chinese herbal medicine quality, it is a requisite technical process in Chinese herbal medicine processing, it is in close relations that dry and Chinese medicine are produced, and dry method will directly affect the quality of product.
The bark of eucommia is the dry bark of the Eucommiaceae plant bark of eucommia, the effect with filling liver kidney, strengthening the bones and muscles, it is the Chinese medicine of medicine-food two-purpose, be rich in the Phenylpropanoid Glycosides classes such as chlorogenic acid, the iridoidses such as Geniposidic acid, geniposide, peach skin coral glycosides, the lignanoids such as Pinoresinol diglucoside, the plurality of active ingredients such as flavonoids such as rutin.
Being dried of the bark of eucommia that < < Chinese pharmacopoeia > > (2010 editions) records is: strip 4～June, scrape off tertia, " sweating " to the endothelium of banking up is puce, dries.
The freeze-drying of prior art is to get the direct freeze-drying of fresh medicine, and object is to preserve to greatest extent fresh the effective elements of the medicine.The bark of eucommia prepared by the present invention, various active component content is high, treatment hypertension better effects if.And product is non-friable, storage, transportation easily keep medicine materical crude slice shape
Below by test example, further illustrate usefulness of the present invention, test example is intended to further illustrate usefulness of the present invention, but not limitation of the present invention.
To scrape off tertia with a collection of fresh bark of eucommia, process by the following method.
1) dry the bark of eucommia " sweating " to the endothelium of banking up and be puce, dry.
2) the freeze-drying bark of eucommia is refrigerated to below-20 ℃, is evacuated to below drying chamber pressure 30Pa, and heating sublimation, the temperature of distillation is controlled at below 40 ℃, and the temperature of resolution phase should be controlled at below 45 ℃, to dry.
3) freeze-drying to the distillation of banking up finishes the bark of eucommia " sweating " to the endothelium of banking up and is puce, is refrigerated to below-20 ℃, is evacuated to below drying chamber pressure 30Pa, heating sublimation, the temperature of distillation is controlled at below 40 ℃, when the pressure drop of freeze drying box is when approaching the pressure of freezer unit, and end.
One, the dry bark of eucommia active component comparison of distinct methods
1, key instrument and equipment
LC-20A high performance liquid chromatograph; UV-5300PC type ultraviolet-uisible spectrophotometer; AG135 type 100,000/electronic balance, freeze dryer.
2, reagent: reference substance chlorogenic acid, geniposide, rutin, caffeic acid are all purchased from Nat'l Pharmaceutical & Biological Products Control Institute, and peach skin coral glycosides, Pinoresinol diglucoside, Geniposidic acid provide by Shandong Traditional Chinese Medicine University.Acetonitrile (chromatographically pure, U.S. Tedia company); Phosphoric acid (chromatographically pure, Ke Miou chemical reagent development centre, Tianjin).
3, test method
Accurately take each sample appropriate, the ethanol with 60% infiltrates after 12h, then uses ultrasonic wave assisted extraction 1h, is filtered in 100mL volumetric flask, repeats 2 times, and merging filtrate, is settled to scale with 60% ethanol, and filtrate is crossed 45 μ m filter membranes, and extract is standby.
1) high effective liquid chromatography for measuring chlorogenic acid chromatographic condition: chromatographic column Dimamonsil C18(250mm * 4.6mm, 5 μ m); Mobile phase methanol: water=35: 75; Flow velocity 1.0mL/min detects wavelength 240nm; Sampling volume 20 μ L; 25 ℃ of temperature.
2) high effective liquid chromatography for measuring Geniposidic acid chromatographic condition: chromatographic column Dimamonsil C 18 (250 mm x 4.6,5 μ m); Flow velocity 1.0 mL/min; Detect wavelength 240nm; Sampling volume 20 μ L; 25 ℃ of temperature; Binary geopressure gradient elution time program: during 0min, methyl alcohol: 0.001% phosphoric acid solution=22:78; During 15 min, methyl alcohol): 0.001% phosphoric acid solution=30:70; During 35 min, methyl alcohol: 0.001% phosphoric acid solution=22: 78; During 40min, sampling finishes.
3) aluminum nitrate one natrium nitrosum colorimetric method for determining general flavone is accurately drawn appropriate extract in 10 mL volumetric flasks, adds containing 5%NaNO
2the aqueous solution 0.3 mL, shakes up, standing 6min; Add again (the N0 containing 10%Al
3)
3the aqueous solution 0.3 mL, shakes up, standing 6min; Add again containing 1.0mol/L NaOH aqueous solution 4mL, shake up standing 15min; With distilled water, be settled to scale.In the interscan of 400-600nm wave-length coverage, determine that maximum absorption wavelength is 506nm.
4) paradime thylaminobenzaldehyde determination of color peach skin coral glycosides is accurately drawn appropriate extract in 10 mL colorimetric cylinders, adds successively 95% ethanol 2.5 mL, Epstahl reagent 1.7 mL, and 20% hydrochloric acid 0.5 mL, then be settled to scale with distilled water.Be placed in water-bath and at 75 ℃, heat 20min and develop the color, take out after cooling 10min, take reagent blank as reference, in the interscan of 500-700nm wave-length coverage, determine that maximum absorption wavelength is 596nm.
4, calibration curve
According to said method, respectively chlorogenic acid, Geniposidic acid, general flavone and peach skin coral glycosides standard specimen are measured drawing standard curve.
5, results and analysis: result is as table 1.
Active constituent content result (%) in the dry bark of eucommia of table 1 distinct methods
By table 1, found out, the fresh bark of eucommia " sweating " to the endothelium of banking up is puce, and it is high that freeze-drying to distillation finishes plurality of active ingredients content, and then known clinical efficacy is good.
Three, the dry eucommia bark depressor effect comparison of distinct methods
1, material
1.1 key instrument rat computer blood pressure cardiotachometers, four lead physiograph.
1.2 animal spontaneous hypertensive rats (SHR), are all male 10 week age, body weight (223.5 ± 23) g, and blood pressure is all greater than 20kPa.
1.3 prepare liquid gets respectively each sample and is cut into silk, extracting in water 3 times, and amount of water is respectively 10,6,6 times of medicinal material weight, and extraction time is 1.5,1,1h, merges extract, concentrates and is settled to every milliliter and be equivalent to crude drug 0.25g, obtains.
2, method and result
2.1 animal models are got rat feeding in constant temperature observation ward, room temperature (21 ± 2) ℃, artificial light 12 hd-1, freely drink water, feeding with 21% high protein feed, measure blood pressure after 1 week, is spontaneous hypertensive rat higher than 22.7 kPa persons, it is divided into above each Eucommia Samples group and hypertension group, 8 every group at random.Each medication group is respectively with 1.12gkg-1 gavage, every day 2 times, continuously 10d; 8 of normal rats, with hypertension group with amount distilled water gavage.
2h after the mensuration rat last administration of 2.2 blood pressures, heart rate, adopts the indirect measuring cell of non-invasive to measure arteria caudalis blood pressure, the heart rate of rat under waking state.Before formal measurement, pressure measurement training every day is 1 time, and 5d altogether conforms, after blood pressure stabilization, starts experiment and observe until rat.Before pressure measurement, rat is put into after (37 ± 1) ℃ electrothermostat preheating 15min, measure rat tail artery systolic pressure (SBP) and heart rate (HR), duplicate measurements 3 times.The impact of the dry bark of eucommia of distinct methods on SHR blood pressure, heart rate.The results are shown in Table 2.
The eucommia bark depressor effect that table 2 distinct methods is dry
| Grouping | Dosage | SBP(kPa) | SR (inferior min -1) |
| Normal group | —— | 15.07±0.68 ※※ | 354±9.64 ※※ |
| Hypertension group | —— | 22.93±1.65 | 486±15.16 |
| Dry | 1.12 | 18.24±0.83 ※ | 386±15.72 ※※ |
| Freeze-drying | 1.12 | 19.07±1.10 | 4.23±14.65 |
| Freeze-drying to the distillation of banking up finishes | 1.12 | 16.82±1.14 ※※ | 359±12.41 ※※ |
From table 2, the dry bark of eucommia of distinct methods has impact in various degree to the blood pressure of animal used as test and heart rate, and freeze-drying to the distillation of wherein banking up finishes the hypotensive effect optimum of the bark of eucommia.
Four, the dry bark of eucommia friability comparison of distinct methods
1, instrument friability somascope, assay balance, hair-dryer.
2, inspection method
The rotating speed that regulates instrument before 2.1 adjusting instrument speed tests is per minute 25 to turn ± 1 turn, and setting test period is 4 minutes, and the total degree of rotary drum is 100 times.
10 of test sample medicine materical crude slice are got in the each test of the amount of taking of 2.2 test samples, with hair-dryer, blow away surperficial powder, precise weighing.
2.3 check
Test sample after above-mentioned weighed weight is put in cylinder, started motor and rotate 100 times.After rotation finishes, check test sample shatter number, then blow away after powder with hair-dryer, accurate claim kind, be the weight of less loss with the difference of the amount of taking, calculate percentage.
3, result, is shown in 3.
Table 3 different dry drying method bark of eucommia friability
| ? | Shatter (%) | Less loss amount (%) |
| Dry | Nothing | 0.35 |
| Freeze-drying | 20 | 4.9 |
| Freeze-drying to the distillation of banking up finishes | 10 | 1.32 |
Table 3 result is known, and the freeze-drying of banking up finishes the bark of eucommia to distillation, and antivibration wear resistant ability is better than the freeze-drying bark of eucommia, and product is non-friable, and storage, transportation easily keep medicine materical crude slice shape, constant product quality.
Summary of the invention
The drying means that the object of this invention is to provide a kind of bark of eucommia, the bark of eucommia that the method is dry, plurality of active ingredients content is high, and clinical efficacy is better.
Another object of the present invention is to provide the application of the bark of eucommia of the present invention, is used for the treatment of hypertension clinical efficacy better.
The object of the present invention is achieved like this:
A drying means for the bark of eucommia, is characterized in that: get the fresh bark of eucommia, scrape off tertia, " sweating " to the endothelium of banking up is puce, and freeze-drying to distillation finishes.
The drying means of a kind of bark of eucommia of the present invention, is characterized in that: it is to be refrigerated to below-20 ℃ that freeze-drying to distillation finishes, be evacuated to below drying chamber pressure 30Pa, and heating sublimation, the temperature of distillation is controlled at below 40 ℃, and freeze-drying to distillation finishes.
A kind of judgement of distillation of the present invention in finishing by the following method 1. condenser temperature drops to the state before distillation; 2. the pressure drop of freeze drying box is to the pressure that approaches freezer unit.
So far completed the present invention, the drying means of a kind of bark of eucommia of the present invention, is different from the freeze-drying of prior art.
The specific embodiment
embodiment 1
Get the fresh bark of eucommia, scrape off tertia, " sweating " to the endothelium of banking up is puce, is refrigerated to-20 ℃, is evacuated to drying chamber pressure 30Pa, heating sublimation, and the temperature of distillation is controlled at below 40 ℃, during state before condenser temperature drops to distillation, finishes.
embodiment 2
Get the fresh bark of eucommia, scrape off tertia, " sweating " to the endothelium of banking up is puce, is refrigerated to-28 ℃, is evacuated to drying chamber pressure 50Pa, heating sublimation, and the temperature of distillation is controlled at 50 ℃, when the pressure drop of freeze drying box is when approaching the pressure of freezer unit, finishes.
embodiment 3
Get the fresh bark of eucommia, scrape off tertia, " sweating " to the endothelium of banking up is puce, is refrigerated to-28 ℃, is evacuated to drying chamber pressure 50Pa, heating sublimation, and the temperature of distillation is controlled at 50 ℃, to distillation end.
embodiment 4
Get the fresh bark of eucommia, scrape off tertia, " sweating " to the endothelium of banking up is puce, is refrigerated to-25 ℃, is evacuated to drying chamber pressure 60Pa, starts heater switch, promotes distillation, and the temperature of distillation should be controlled at 40 ℃, to distilling, finishes.
embodiment 5
Get the fresh bark of eucommia, scrape off tertia, " sweating " to the endothelium of banking up is puce, is refrigerated to-32 ℃, is evacuated to drying chamber pressure 60Pa, starts heater switch, promotes distillation, and the temperature of distillation should be controlled at 40 ℃, to distilling, finishes.
embodiment 6
Get the fresh bark of eucommia, scrape off tertia,, " sweating " to the endothelium of banking up is puce, is refrigerated to-32 ℃, is evacuated to drying chamber pressure 60Pa, starts heater switch, promotes distillation, and the temperature of distillation should be controlled at 40 ℃, to distilling, finishes.
embodiment 7
Get fresh folium cortex eucommiae, pile and be vexedly puce to endothelium, be refrigerated to-20 ℃, be evacuated to drying chamber pressure 30Pa, heating sublimation, the temperature of distillation is controlled at below 40 ℃, finishes to distillation.
embodiment 8
Get fresh folium cortex eucommiae, pile and be vexedly puce to endothelium, be refrigerated to-28 ℃, be evacuated to drying chamber pressure 50Pa, heating sublimation, the temperature of distillation is controlled at 50 ℃, finishes to distillation.
embodiment 9
Get fresh folium cortex eucommiae, pile and be vexedly puce to endothelium, be refrigerated to-30 ℃, be evacuated to drying chamber pressure 50Pa, heating sublimation, the temperature of distillation is controlled at 50 ℃, finishes to distillation.
Claims (2)
1. a freeze drying process for the bark of eucommia, is characterized in that: get the fresh bark of eucommia, " sweating " to the endothelium of banking up is puce, and freeze-drying to distillation finishes.
2. according to the freeze drying process of a kind of bark of eucommia of claim 1, it is characterized in that: freeze-drying is to be refrigerated to below-20 ℃, be evacuated to below drying chamber pressure 30Pa, heating sublimation, the temperature of distillation is controlled at below 40 ℃, to distillation end.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112007068A (en) * | 2020-09-16 | 2020-12-01 | 芜湖晋诚农业科技股份有限公司 | Fermentation method of traditional Chinese medicine eucommia bark |
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| JP2010054064A (en) * | 2008-08-26 | 2010-03-11 | Kyowa Shinku Gijutsu Kk | Freeze drying method and freeze drying apparatus |
| CN102716175A (en) * | 2012-07-04 | 2012-10-10 | 上海玉成干燥设备有限公司 | Superfine eucommia ulmoides powder and preparation method thereof |
| TW201350776A (en) * | 2012-06-08 | 2013-12-16 | Ivorist Internat Co Ltd | Freeze-drying method |
| CN103948652A (en) * | 2014-05-15 | 2014-07-30 | 济南康众医药科技开发有限公司 | Method for drying lucid ganoderma |
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2014
- 2014-08-25 CN CN201410418477.1A patent/CN104142046A/en active Pending
Patent Citations (5)
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| JP2010054064A (en) * | 2008-08-26 | 2010-03-11 | Kyowa Shinku Gijutsu Kk | Freeze drying method and freeze drying apparatus |
| TW201350776A (en) * | 2012-06-08 | 2013-12-16 | Ivorist Internat Co Ltd | Freeze-drying method |
| CN102716175A (en) * | 2012-07-04 | 2012-10-10 | 上海玉成干燥设备有限公司 | Superfine eucommia ulmoides powder and preparation method thereof |
| CN103948652A (en) * | 2014-05-15 | 2014-07-30 | 济南康众医药科技开发有限公司 | Method for drying lucid ganoderma |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112007068A (en) * | 2020-09-16 | 2020-12-01 | 芜湖晋诚农业科技股份有限公司 | Fermentation method of traditional Chinese medicine eucommia bark |
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