CN104147083A - Application of freeze-drying technology in drying of eucommia ulmoides leaves - Google Patents
Application of freeze-drying technology in drying of eucommia ulmoides leaves Download PDFInfo
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- CN104147083A CN104147083A CN201410418490.7A CN201410418490A CN104147083A CN 104147083 A CN104147083 A CN 104147083A CN 201410418490 A CN201410418490 A CN 201410418490A CN 104147083 A CN104147083 A CN 104147083A
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- folium eucommiae
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- eucommia ulmoides
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Abstract
The invention relates to an application of a freeze-drying technology in drying of eucommia ulmoides leaves. A method includes following steps: performing a freeze-drying process to fresh eucommia ulmoides leaves until sublimation is finished; taking out the eucommia ulmoides leaves; stacking the eucommia ulmoides leaves until the eucommia ulmoides leaves "sweats" and are purple-brown in color; and performing a drying process. Prepared eucommia ulmoides leaves are high in contents of various active ingredients and good in clinical effects.
Description
Invention field
The present invention relates to medicine, the particularly application of freeze drying technology in Folium Eucommiae is dry, belongs to medical technical field.
Background technology
Folium Eucommiae is the dried leaves of the Eucommiaceae plant Cortex Eucommiae, the effect with invigorating the liver and kidney, bone and muscle strengthening, it is the Chinese crude drug of medicine-food two-purpose, be rich in the Phenylpropanoid Glycosides classes such as chlorogenic acid, the iridoidses such as Geniposidic acid, geniposide, aucubin, the lignanoids such as pinoresinol diglucoside, the plurality of active ingredients such as flavonoid such as rutin.But Folium Eucommiae is plucked fresh fortune difficulty, so its drying mode, directly have influence on quality and the deep development of medical material.
< < Chinese Pharmacopoeia > > (2010 editions one) records: Folium Eucommiae is the dried leaves of the Eucommiaceae plant Cortex Eucommiae.Summer, autumn gathered when two seasons, branch and leaf were luxuriant, dried or oven drying at low temperature.
Summary of the invention
The object of this invention is to provide the dry new method of a kind of Cortex Eucommiae, the Folium Eucommiae that the method is dry, plurality of active ingredients content is high.
The object of the present invention is achieved like this:
The application of freeze drying technology in Folium Eucommiae is dry, gets fresh Folium Eucommiae, piles vexedly to being brown, and lyophilizing to distillation finishes.
The application of freeze drying technology of the present invention in Folium Eucommiae is dry, is characterized in that: it is to be refrigerated to below-10 ℃ that lyophilizing to distillation finishes, and drying chamber pressure is controlled at below 30Pa, and sublimation temperature is controlled at below 40 ℃, and extremely 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 cryoprobe.
So far completed the present invention, the application of freeze drying technology of the present invention in Folium Eucommiae is dry, is different from the lyophilizing of prior art.The freeze-drying process of prior art mainly can be divided into primary drying (sublimation drying), and redrying (adsorption stripping and dry) is to dry.The dry run pumpdown time is long, and energy consumption is high.The present invention is application freeze drying technology, and lyophilizing to distillation finishes, and takes out, without redrying process.The dry run pumpdown time is short, and energy consumption is low; Dry products is non-friable, easily preserves; Folium Eucommiae active constituent content that the more important thing is preparation is high, and clinical effectiveness is good.
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 Eucommiae, process by the following method.
1) dry Folium Eucommiae: fresh Folium Eucommiae, dries.
2) pile vexed lyophilizing to distillation and finish Folium Eucommiae: fresh Folium Eucommiae, pile vexedly to being brown, be refrigerated to-20 ℃, be evacuated to drying chamber pressure 30Pa, subliming by heating, the temperature of distillation should be controlled at below 40 ℃, during state before condenser temperature drops to distillation, obtain.
3) lyophilizing Folium Eucommiae: fresh Folium Eucommiae, is refrigerated to-20 ℃; Reach after cryogenic temperature, be evacuated to below drying chamber pressure 30Pa, start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃, to dry.
One, the dry Folium 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 Fructus Persicae skin Corallium Japonicum Kishinouye 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 ultrasound 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 extracting solution 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, methanol: 0.001% phosphoric acid solution=22:78; During 15min, methanol: 0.001% phosphoric acid solution=30:70; During 35 min, methanol: 0.001% phosphoric acid solution=22:78; During 40min, sampling finishes.
3) aluminum nitrate one sodium nitrite colorimetric method for determining total flavones is accurately drawn appropriate extracting solution 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 Fructus Persicae skin Corallium Japonicum Kishinouye glycosides is accurately drawn appropriate extracting solution in 10mL color comparison tube, 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, standard curve
According to said method, respectively chlorogenic acid, Geniposidic acid, total flavones and Fructus Persicae skin Corallium Japonicum Kishinouye 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 Cortex Eucommiae that distinct methods processes, result is as table 1.
Active constituent content result (%) in the dry Folium Eucommiae of table 1 distinct methods
By table 1, learnt, Folium Eucommiae is piled vexed lyophilizing to distillation and is finished rear being dried, and active constituent content is apparently higher than " drying Folium Eucommiae " and " lyophilizing Folium Eucommiae ", and then known clinical efficacy is good.
Two, the dry Folium 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 medicinal liquid gets respectively " drying Folium Eucommiae ", " pile vexed lyophilizing to distillation and finish Folium Eucommiae ", " lyophilizing Folium Eucommiae ", extracting in water 3 times, amount of water is respectively 10,6,6 times of medical material weight, extraction time is 1.5,1,1h, merge extractive liquid,, concentrate and be settled to every milliliter and be equivalent to crude drug 0.25g, obtain.
2, method and result
2.1 animal models are got rat feeding in constant temperature observation ward, room temperature (21 ± 2) ℃, artificial lighting 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 to " drying Folium Eucommiae group ", " pile vexed lyophilizing to distillation and finish Folium Eucommiae group ", " lyophilizing Folium Eucommiae group " 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 commensurability 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 laboratory observation 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), repeated measure 3 times.The impact of the dry Cortex Eucommiae of distinct methods on SHR blood pressure, heart rate, the results are shown in Table 2.
The Folium Eucommiae antihypertensive 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 group | 1.12 | 18.24±0.83 | 386±15.72 |
| Pile vexed lyophilizing to the end group that distils | 1.12 | 16.35±0.64 | 355±14.61 |
| Lyophilizing group | 1.12 | 18.94±1.73 | 424±14.47 |
From table 2, " Folium Eucommiae lyophilizing finishes the vexed dry hypotensive effect of rear heap to distillation and is better than " drying Folium Eucommiae " and " lyophilizing Folium Eucommiae ", illustrates that the dry eucommia bark depressor of the inventive method is effective.
Three, the dry Folium Eucommiae friability comparison of distinct methods
1, instrument friability somascope, analytical 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.
Taking of 2.2 test samples measures test sample, with hair-dryer, blows away surperficial powder, gets 10g, 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, then blow away after powder with hair-dryer, precise weighing, is the weight of less loss with the difference of the amount of taking, and calculates percentage ratio.
3, result, is shown in 3.
Table 3 distinct methods is dried Folium Eucommiae friability result (%)
| Sample | Dry | Lyophilizing | Piling vexed lyophilizing to distillation finishes |
| Less loss amount (%) | 1.36 | 6.47 | 1.85 |
Table 3 result is known, and Folium Eucommiae friability of the present invention is low, and product is non-friable, and storage, transportation easily keep decoction pieces shape, constant product quality.
The specific embodiment
embodiment 1
Get fresh Folium Eucommiae, pile vexed 1 day, through checking, be brown, be refrigerated to-10 ℃, be evacuated to drying chamber pressure 30Pa, subliming by heating, sublimation temperature is controlled at 40 ℃, and during state before condenser temperature drops to distillation, distillation finishes, and obtains.
embodiment 2
Get fresh Folium Eucommiae, pile vexed 3 days, through checking, be brown, be refrigerated to-25 ℃, be evacuated to drying chamber pressure 45Pa, subliming by heating, the temperature of distillation is controlled at 40 ℃, and when the pressure drop of freeze drying box is when approaching the pressure of cryoprobe, distillation finishes, and obtains.
embodiment 3
Get fresh Folium Eucommiae, pile vexedly to being brown, be refrigerated to-32 ℃, be evacuated to drying chamber pressure 60Pa, subliming by heating, the temperature of distillation should be controlled at 40 ℃, finishes to distillation, obtains.
embodiment 4
Get fresh Folium Eucommiae, pile vexedly to being brown, be refrigerated to-28 ℃, be evacuated to drying chamber pressure 60Pa, subliming by heating, the temperature of distillation should be controlled at 40 ℃, finishes to distillation, obtains.
embodiment 5
Get the fresh Cortex Eucommiae, pile vexedly to being brown, be refrigerated to-30 ℃, be evacuated to drying chamber pressure 55Pa, subliming by heating, the temperature of distillation is controlled at 40 ℃, finishes to distillation, obtains.
Claims (3)
1. the application of freeze drying technology in Folium Eucommiae is dry, is characterized in that: get fresh Folium Eucommiae, pile vexedly to being brown, lyophilizing to distillation finishes.
2. the application in Folium Eucommiae is dry according to the freeze drying technology of claim 1, is characterized in that: it is to be refrigerated to below-10 ℃ that lyophilizing to distillation finishes, and drying chamber pressure is controlled at below 30Pa, and sublimation temperature is controlled at below 40 ℃, and extremely distillation finishes.
3. the application in Folium Eucommiae is dry according to the freeze drying technology of claim 1 or claim 2, is characterized in that: a kind of judgement in distillation end 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 cryoprobe.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108379333A (en) * | 2018-03-17 | 2018-08-10 | 贵阳中医学院 | A kind of processing method of Eucommia ulmoides |
| CN113230301A (en) * | 2021-04-29 | 2021-08-10 | 赵艳 | Eucommia leaf pretreatment method for extracting pinoresinol diglucoside from eucommia leaves |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 CN201410418490.7A patent/CN104147083A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 (4)
| Title |
|---|
| 兰小艳: "杜仲叶中绿原酸的研究进展", 《中国农学通报》 * |
| 姚静: "《药物冻干制剂技术的设计及应用》", 30 June 2007, 中国医药科技出版社 * |
| 程文亮: "《浙江丽水药物志》", 30 April 2014, 中国农业科学技术出版社 * |
| 黄达芳: "《实用中药鉴定学》", 31 August 2004, 科学出版社 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108379333A (en) * | 2018-03-17 | 2018-08-10 | 贵阳中医学院 | A kind of processing method of Eucommia ulmoides |
| CN113230301A (en) * | 2021-04-29 | 2021-08-10 | 赵艳 | Eucommia leaf pretreatment method for extracting pinoresinol diglucoside from eucommia leaves |
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Application publication date: 20141119 |