CN104154710A - Freeze-drying method of Eucommia ulmoides leaves - Google Patents
Freeze-drying method of Eucommia ulmoides leaves Download PDFInfo
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- CN104154710A CN104154710A CN201410418569.XA CN201410418569A CN104154710A CN 104154710 A CN104154710 A CN 104154710A CN 201410418569 A CN201410418569 A CN 201410418569A CN 104154710 A CN104154710 A CN 104154710A
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- cortex eucommiae
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- folium cortex
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Abstract
The invention relates to a freeze-drying method of Eucommia ulmoides leaves. The freeze-drying method is characterized by comprising the steps of taking the fresh Eucommia ulmoides leaves, piling the Eucommia ulmoides leaves in a smouldering mode until the Eucommia ulmoides leaves become brown, and then drying the Eucommia ulmoides leaves in a freezing mode. The content of various active ingredients of the prepared Eucommia ulmoides leaves is high, and the effect of treating the high blood pressure is good.
Description
Invention field
The present invention relates to medicine method for making, particularly a kind of freeze drying process of folium cortex eucommiae, 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 quality will directly affect the quality of product.
< < Chinese pharmacopoeia > > (2010 editions one) records: folium cortex eucommiae is the dry leaf of the Eucommiaceae plant bark of eucommia.Summer, autumn gathered when two seasons, branches and leaves were luxuriant, dried or low temperature drying.We find that the dry folium cortex eucommiae active constituent content of this method is low, and clinical effectiveness is poor.
Summary of the invention
The freeze drying process that the object of this invention is to provide a kind of folium cortex eucommiae, the folium cortex eucommiae that the method is dry, the drying means that plurality of active ingredients content records apparently higher than < < Chinese pharmacopoeia > > (2010 editions).
Another object of the present invention is to provide a kind of application of freeze-drying folium cortex eucommiae, is used for the treatment of hypertension clinical efficacy better.
The object of the present invention is achieved like this:
A freeze drying process for folium cortex eucommiae, is characterized in that: get fresh folium cortex eucommiae, pile vexed to being brown, freeze-drying.
The freeze drying process of a kind of folium cortex eucommiae of the present invention, is characterized in that: freeze-drying is to be refrigerated to below-20 ℃, be evacuated to below drying chamber pressure 30Pa, and heating sublimation, the temperature of distillation is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
The application of folium cortex eucommiae prepared by the freeze drying process of a kind of folium cortex eucommiae of the present invention, is characterized in that: be used for the treatment of hypertension.
So far completed the present invention, the freeze drying process of a kind of folium cortex eucommiae of the present invention, is different from the freeze-drying of prior art.The freeze-drying that has technology 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, and we find to get fresh folium cortex eucommiae, and directly its various active component content of freeze-drying is not high.
The freeze drying process of a kind of folium cortex eucommiae of the present invention, it is the vexed rear freeze-drying of heap, the folium cortex eucommiae of preparation, the drying means that various active component content records apparently higher than < < Chinese pharmacopoeia > > (2010 editions), also higher than the direct freeze-drying of fresh folium cortex eucommiae.Treatment hypertension better effects if.
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, with a collection of fresh folium cortex eucommiae, process by the following method.
1) dry folium cortex eucommiae: get fresh folium cortex eucommiae, dry.
2) pile vexed freeze-drying folium cortex eucommiae: get fresh folium cortex eucommiae, pile vexedly to being brown, be refrigerated to below-20 ℃, be evacuated to below drying chamber pressure 30Pa, heating sublimation, sublimation temperature is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
3) freeze-drying folium cortex eucommiae: get fresh folium cortex eucommiae, be refrigerated to below-20 ℃, be evacuated to below drying chamber pressure 30Pa, heating sublimation, sublimation temperature is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
One, the dry folium cortex eucommiae 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 1.0mL/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
2aqueous solution 0.3mL, shakes up, standing 6min; Add again (the N0 containing 10%Al
3)
3aqueous solution 0.3mL, 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
Adopt above-mentioned experimental technique to detect the content of various active composition in the folium cortex eucommiae skin that distinct methods processes, result is as table 1.
Active constituent content result (%) in the dry folium cortex eucommiae of table 1 distinct methods
By table 1, learnt, pile the content of vexed rear freeze-drying Chlorogenic Acid in Eucommia ulmoides Oliv. Leaves, Geniposidic acid, general flavone and aucubin apparently higher than drying folium cortex eucommiae and freeze-drying folium cortex eucommiae, and then known clinical efficacy is good.
Two, the dry folium cortex eucommiae antihypertensive 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, 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 at random and dries folium cortex eucommiae group, pile vexed freeze-drying folium cortex eucommiae group, freeze-drying folium cortex eucommiae and hypertension group, 8 every group.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 dry folium cortex eucommiae of distinct methods the results are shown in Table 2 to the impact of SHR blood pressure, heart rate.
The folium cortex eucommiae antihypertensive effect that table 2 distinct methods is dry
| Grouping | Dosage (gkg -1) | 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 folium cortex eucommiae | 1.12 | 19.16±1.10 | 441±14.15 |
| Pile vexed freeze-drying folium cortex eucommiae | 1.12 | 16.82±1.14 | 359±12.41 |
| Freeze-drying folium cortex eucommiae | 1.12 | 18.92±1.64 | 386±14.57 |
From table 2, the dry folium cortex eucommiae of distinct methods has impact in various degree to the blood pressure of animal used as test and heart rate, the hypotensive effect of wherein piling vexed freeze-drying folium cortex eucommiae group is better than drying folium cortex eucommiae and freeze-drying folium cortex eucommiae group, illustrates that the dry folium cortex eucommiae antihypertensive effect of the inventive method is good.
The specific embodiment
embodiment 1
Get fresh folium cortex eucommiae, pile vexedly to being brown, be refrigerated to-20 ℃, be evacuated to drying chamber pressure 30Pa, heating sublimation, the temperature of distillation is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 2
Get fresh folium cortex eucommiae, pile vexedly to being brown, be refrigerated to-28 ℃, be evacuated to drying chamber pressure 50Pa, heating sublimation, the temperature of distillation is controlled at 50 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 3
Get fresh folium cortex eucommiae, pile vexedly to being brown, be refrigerated to-28 ℃, be evacuated to drying chamber pressure 50Pa, heating sublimation, the temperature of distillation is controlled at 50 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 4
Get fresh folium cortex eucommiae, pile vexedly to being brown, be refrigerated to-25 ℃, be evacuated to drying chamber pressure 60Pa, start heater switch, promote distillation, the temperature of distillation should be controlled at 40 ℃, finishes to distillation, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 5
Get fresh folium cortex eucommiae, pile vexedly to being purple, be refrigerated to-32 ℃, be evacuated to drying chamber pressure 60Pa, start heater switch, promote distillation, the temperature of distillation should be controlled at 40 ℃, finishes to distillation, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 6
Get fresh folium cortex eucommiae, pile vexedly to being brown, be refrigerated to-32 ℃, be evacuated to drying chamber pressure 60Pa, start heater switch, promote distillation, the temperature of distillation should be controlled at 40 ℃, finishes to distillation, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 7
Get fresh folium cortex eucommiae, pile vexed 2 days, watch and be brown, be refrigerated to-28 ℃, be evacuated to drying chamber pressure 50Pa, heating sublimation, the temperature of distillation is controlled at 50 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
embodiment 8
Get fresh folium cortex eucommiae, pile vexed 4 days, watch and be brown, be refrigerated to-25 ℃, be evacuated to drying chamber pressure 60Pa, start heater switch, promote distillation, the temperature of distillation should be controlled at 40 ℃, to distilling, finishes, and resolution temperature is controlled at below 45 ℃, to dry.
Claims (3)
1. a freeze drying process for folium cortex eucommiae, is characterized in that: get fresh folium cortex eucommiae, pile vexed to being brown, freeze-drying.
2. according to the freeze drying process of a kind of folium cortex eucommiae of claim 1, it is characterized in that: freeze-drying is to be refrigerated to below-20 ℃, is evacuated to below drying chamber pressure 30Pa, heating sublimation, the temperature of distillation is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry.
3. the application of the folium cortex eucommiae that prepared by the present invention, is characterized in that: be used for the treatment of hypertension.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09152268A (en) * | 1995-11-30 | 1997-06-10 | Liquid Gas:Kk | Freeze dryer |
| CN103055022A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Method for processing rehmannia and application for rehmannia in preparation for medicine |
| CN103948638A (en) * | 2014-05-15 | 2014-07-30 | 济南康众医药科技开发有限公司 | Drying method of medical fungi |
| CN103977041A (en) * | 2014-05-15 | 2014-08-13 | 济南康众医药科技开发有限公司 | Drying method of ganoderma applanatum pat |
-
2014
- 2014-08-25 CN CN201410418569.XA patent/CN104154710A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH09152268A (en) * | 1995-11-30 | 1997-06-10 | Liquid Gas:Kk | Freeze dryer |
| CN103055022A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Method for processing rehmannia and application for rehmannia in preparation for medicine |
| CN103948638A (en) * | 2014-05-15 | 2014-07-30 | 济南康众医药科技开发有限公司 | Drying method of medical fungi |
| CN103977041A (en) * | 2014-05-15 | 2014-08-13 | 济南康众医药科技开发有限公司 | Drying method of ganoderma applanatum pat |
Non-Patent Citations (3)
| Title |
|---|
| 吕强: "杜仲总木脂素及松脂醇二葡萄糖苷的提取纯化研究", 《吉首大学硕士学位论文》 * |
| 国家药典委员会编: "《中华人民共和国药典 2010年版 1部 》", 31 January 2010 * |
| 范青生等: "《保健食品配方原理与依据》", 31 January 2007, 中国医药科技出版社 * |
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Address after: 250014 No. 81, Shandong Road, thousand Buddha, Lixia District, Ji'nan, Shandong Applicant after: Jinan Kangzhong Medicin Science & Technology Co., Ltd. Address before: Lixia District Hospital in Shandong province Ji'nan City Road 250014 No. 19 No. 4 West of Shandong Academy of Sciences Applicant before: Jinan Kangzhong Medicin Science & Technology Co., Ltd. |
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Inventor after: Li Jiawei Inventor after: Ma Yukui Inventor after: Guo Qinghua Inventor after: Feng Lijuan Inventor before: Niu Fengju Inventor before: Ma Yukui Inventor before: Guo Qinghua Inventor before: Feng Lijuan |
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Application publication date: 20141119 |