CN104147225A - Freeze-dried rehmannia glutinosa used as high-bioavailability decocting pieces - Google Patents
Freeze-dried rehmannia glutinosa used as high-bioavailability decocting pieces Download PDFInfo
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- CN104147225A CN104147225A CN201410418936.6A CN201410418936A CN104147225A CN 104147225 A CN104147225 A CN 104147225A CN 201410418936 A CN201410418936 A CN 201410418936A CN 104147225 A CN104147225 A CN 104147225A
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Abstract
The invention relates to freeze-dried rehmannia glutinosa used as high-bioavailability decocting pieces. The invention is characterized in that freeze-dried rehmannia glutinosa decocting pieces is higher than fresh rehmannia glutinosa in bioavailability and can be processed into raw rehamnnia glutinosa and prepared rehmannia glutinosa.
Description
Invention field
The present invention relates to medicine, particularly lyophilizing Radix Rehmanniae, as the high decoction pieces of bioavailability, belongs to medical technical field.
Background technology
Freeze drying technology is also widely application in the Chinese crude drug Preparation process of China, in the Chinese crude drugs such as Radix Ginseng, Radix Panacis Quinquefolii, Cordyceps, Rhizoma Dioscoreae, Fructus Lycii, Cornu Cervi Pantotrichum, all appears in the newspapers.Freeze drying technology can be preserved the activity of effective medicinal components to greatest extent, and effective ingredient is higher than the prepared slices of Chinese crude drugs of other dry technology processing.The Chinese traditional medicine biology availability that does not also have at present freeze drying technology to process is better than the bibliographical information of fresh medicine.
Radix Rehmanniae is the fresh or dried root of scrophulariaceae rehmannia glutinosa plant.The main component of Radix Rehmanniae has iridoid (mainly containing catalpol), monoterpene and glycoside thereof, is secondly saccharide, also contains several amino acids, organic acid and inorganic elements.According to bibliographical information, Radix Rehmanniae is in concocting into Radix Rehmanniae and Radix Rehmanniae Preparata process, and change has occurred ingredient, and its pharmacologically active and clinical function also have very big-difference.
The active height of the prepared slices of Chinese crude drugs enters speed in body and degree by effective ingredient and determines, effective ingredient is absorbed fast and amount is how active just high, on the contrary existing problems likely just, and curative effect is just unreliable.
Patent of invention CN201310008813.0 discloses a kind of freeze drying process of fresh ground, and lyophilizing rehmannia catalpol content and Radix Rehmanniae are suitable, apparently higher than Radix Rehmanniae.But do not relate to lyophilizing Radix Rehmanniae and prepare high activity radix rehmanniae.
Summary of the invention
The new purposes that the object of this invention is to provide a kind of lyophilizing Radix Rehmanniae, lyophilizing Radix Rehmanniae is as the high decoction pieces of bioavailability, and bioavailability, higher than Radix Rehmanniae, is more convenient for being processed into Radix Rehmanniae and Radix Rehmanniae Preparata.
The present invention is achieved in that
Lyophilizing Radix Rehmanniae, as the high decoction pieces of bioavailability, is characterized in that: lyophilizing radix rehmanniae bioavailability, higher than Radix Rehmanniae, is more convenient for being processed into Radix Rehmanniae and Radix Rehmanniae Preparata.
Lyophilizing Radix Rehmanniae of the present invention, as the high decoction pieces of bioavailability, is characterized in that: the method for lyophilizing Radix Rehmanniae is: get Radix Rehmanniae, put in freeze dryer, solidification point is controlled between-28～-32 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃, dry end when temperature of charge and heating-up temperature approach.
So far completed the present invention, it provides the new purposes of a kind of lyophilizing Radix Rehmanniae, and lyophilizing Radix Rehmanniae is as the high decoction pieces of bioavailability, and the decoction pieces bioavailability of preparing with lyophilizing Radix Rehmanniae is high, and then known activity is high, and is more convenient for being processed into Radix Rehmanniae and Radix Rehmanniae Preparata.
As well known to those skilled in the art, fresh medicine lyophilizing can be preserved the activity of effective medicinal components to greatest extent, keeps preferably exterior quality, color, the abnormal smells from the patient of medical material.The object of prior art application lyophilizing medical material is to make it active suitable with fresh medicine, with respect to other drying means, active high, rather than makes its activity higher than fresh medicine.We find that lyophilizing rehmannia catalpol content is slightly lower than Radix Rehmanniae, but the decoction pieces catalpol bioavailability of preparing with lyophilizing Radix Rehmanniae is high.Lyophilizing Radix Rehmanniae of the present invention is prepared the decoction pieces that bioavailability is high, and this new purposes has no report.With lyophilizing Radix Rehmanniae, prepare the decoction pieces that bioavailability is high, essence does not lie in lyophilizing Radix Rehmanniae itself, and is how to go to use it, the creative and novelty of new purposes or new object.
Below by test example, usefulness of the present invention is described.
With same plot, Dingyao County, Shandong Province, play the new Radix Rehmanniae piece of soil simultaneously, test.
One, lyophilizing radix rehmanniae and the comparison of Radix Rehmanniae catalpol content
1, prepare sample
1) Radix Rehmanniae: new Radix Rehmanniae tuber soil buries, plastic bag sealing moisturizing;
2) lyophilizing radix rehmanniae: get Radix Rehmanniae, be cut into sheet, put in freeze dryer, solidification point is controlled at-32 ℃; Drying chamber pressure is controlled at below 50Pa; The temperature of China is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃.When temperature of charge and heating-up temperature approach, dry end, takes out, and obtains lyophilizing radix rehmanniae.
2, lyophilizing radix rehmanniae and the comparison of fresh rehmannia catalpol content
Instrument: Shimadzu LC-3A chromatograph, chromatographic condition: chromatographic column YWG-C18,10 μ m, 25cm * 4.6mm.Mobile phase: 0.6% acetonitrile-water.Flow velocity: 1.0mLmin
-1, measure wavelength 210 nm.40 ℃ of column temperatures.
The preparation of sample solution: Radix Rehmanniae is rubbed, and Radix Rehmanniae was pulverized 40 mesh sieves, the Radix Rehmanniae 2.5g(drying of accurately weighed rubbing test 5g Radix Rehmanniae obtains 1g lyophilizing Radix Rehmanniae respectively), lyophilizing radix rehmanniae 0.5g, add methanol 25mL, weigh, supersound process 20min, let cool, mend and weigh, filter.Get subsequent filtrate as need testing solution.
The preparation of reference substance solution: accurately weighed catalpol reference substance 2.87mg, put in 10 mL measuring bottles, add mobile phase and dissolve and be diluted to scale, shake up product solution in contrast.
Precision is drawn reference substance solution 3 μ L respectively, and need testing solution 6 μ L inject hplc determination.In dry product, the results are shown in Table 1.
Table 1 lyophilizing radix rehmanniae and Radix Rehmanniae catalpol content
| ? | Catalpol content (%) |
| Radix Rehmanniae | 6.18 |
| Lyophilizing radix rehmanniae | 5.67 |
Known in Table 1 result, in dry product lyophilizing radix rehmanniae catalpol content slightly lower than Radix Rehmanniae.
Two, lyophilizing radix rehmanniae and the comparison of Radix Rehmanniae bioavailability
Instrument: Shimadzu LC-3A chromatograph, chromatographic condition: chromatographic column YWG-C18,10 μ m, 25cm * 4.6mm.Mobile phase: 0.6% acetonitrile-water.Flow velocity: 1.0mLmin-1, measures wavelength 210 nm.40 ℃ of column temperatures.
The preparation of reference substance solution: with test one.
The preparation of sample solution: Radix Rehmanniae is rubbed; Lyophilizing radix rehmanniae was pulverized 40 mesh sieves, and distilled water adds to 5 times of amounts (drying test 5g Radix Rehmanniae obtains 1g lyophilizing Radix Rehmanniae).
The preparation of rat blood serum after administration: by 30 of Wistar rats, be divided at random 3 groups, blank group, lyophilizing radix rehmanniae group, Radix Rehmanniae group.Administration group dosage is 1.5mL/100g, gavage, and blank group gives same volume distilled water.Fasting 12h before experiment, freely drinks water.After administration 2h, intramuscular injection 10% chloral hydrate (0.3mL/100g) anesthesia, abdominal aortic blood.The standing 1h of blood, the centrifugal 10min of 3000r/min, draws supernatant, puts in-20 ℃ of refrigerators and saves backup.
The processing of serum: the accurate serum 2mL that draws, adds methanol 8mL, vortex vibration 2min, the centrifugal 20min of 3000r/min, get supernatant, it is dry that nitrogen dries up instrument, and mobile phase is dissolved, be settled in 2mL volumetric flask, 0.45 μ m filtering with microporous membrane, for efficient liquid phase chromatographic analysis.
The high performance liquid chromatogram collection of illustrative plates contrast of each serum: high activity radix rehmanniae group and the more blank serum group of Radix Rehmanniae group serum, have more a new chromatographic peak, new chromatographic peak in identical position, illustrates that new chromatographic peak is the characteristic peak of catalpol with catalpol chromatographic peak.
The peak area that compares catalpol in lyophilizing radix rehmanniae group and Radix Rehmanniae group serum, result, high activity radix rehmanniae group peak area is 1.26 times of Radix Rehmanniae group serum peak area.Illustrate that high activity radix rehmanniae is higher than Radix Rehmanniae bioavailability.
Three, lyophilizing radix rehmanniae and Radix Rehmanniae decoction pieces are prepared Radix Rehmanniae Preparata period ratio
1, prepare sample
1) Radix Rehmanniae is prepared Radix Rehmanniae Preparata: get Radix Rehmanniae, according to < < Chinese Pharmacopoeia > > version in 2010, steam method, steam to black profit, writing time, take out, when dry in the sun is slightly dry to crust mucus, cut sheet or piece, 60 ℃ following dry, obtains Radix Rehmanniae Preparata, writing time.
2) lyophilizing radix rehmanniae is prepared Radix Rehmanniae Preparata: Radix Rehmanniae is refrigerated to below-10 ℃, rises to room temperature, take out and slowly to cure to eighty per cant dry, according to < < Chinese Pharmacopoeia > > version in 2010, steam method, steam to black profit, writing time, take out, when dry in the sun is slightly dry to crust mucus, cut sheet or piece, 60 ℃ following dry, dry, obtain Radix Rehmanniae Preparata, writing time.The results are shown in Table 2, table 3.
The different radix rehmanniaes of table 2 steam to the black profit time (hour, %)
| Sequence number | Method for making | Time |
| 1 | Radix Rehmanniae | 8 |
| 2 | Lyophilizing radix rehmanniae | 4 |
Drying time after the different radix rehmanniaes of table 3 steam (hour, %)
| Sequence number | Method for making | Time | Water content |
| 1 | Radix Rehmanniae | 14 | 13.8 |
| 2 | Lyophilizing radix rehmanniae | 10 | 10.3 |
Result finds out, lyophilizing radix rehmanniae is prepared Radix Rehmanniae Preparata, and the process-cycle obviously shortens, and then known, and lyophilizing radix rehmanniae is more convenient for concocting.
The specific embodiment
embodiment 1
Get new Radix Rehmanniae, clean roguing, be cut into the Radix Rehmanniae section of length 5cm; By the sabot of Radix Rehmanniae section, loading amount is 4Kg/ ㎡ left and right; Solidification point is controlled at-28 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃, and when temperature of charge and heating-up temperature approach, dry end, takes out, and cutting, obtains lyophilizing radix rehmanniae.
embodiment 2
Get Radix Rehmanniae, put in freeze dryer, solidification point is controlled at-32 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃, and when temperature of charge and heating-up temperature approach, dry end, takes out, and obtains freeze dried fresh Radix Rehmanniae medical material, makes decoction pieces, obtains lyophilizing radix rehmanniae.
embodiment 3
Get Radix Rehmanniae, put in freeze dryer, solidification point is controlled at-30 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃, and when temperature of charge and heating-up temperature approach, dry end, takes out, and obtains freeze dried fresh Radix Rehmanniae medical material, makes decoction pieces, obtains lyophilizing radix rehmanniae.
embodiment 4
Get Radix Rehmanniae, cut into slices, put in freeze dryer, solidification point is controlled between 29 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃, and when temperature of charge and heating-up temperature approach, dry end, takes out, and obtains lyophilizing radix rehmanniae.
embodiment 5
Get Radix Rehmanniae, cut into slices, put in freeze dryer, solidification point is controlled between 30 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃, and when temperature of charge and heating-up temperature approach, dry end, takes out, and obtains lyophilizing radix rehmanniae.
embodiment 6
Get Radix Rehmanniae, cut into chunks, put in freeze dryer, solidification point is controlled between 31 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃, and when temperature of charge and heating-up temperature approach, dry end, takes out, and obtains lyophilizing radix rehmanniae.
embodiment 7
Get a kind of lyophilizing radix rehmanniae prepared by above embodiment, be crushed to coarse powder, add 4 times of water gagings, 20 ℃ of following stirrings, extract 4 hours, extracting liquid filtering, centrifugal, obtain lyophilizing Radix Rehmanniae extracting solution;
The lyophilizing of lyophilizing Radix Rehmanniae extracting solution, vacuum is-35.0Pa that pre-freeze temperature-40 ℃, are incubated 2 hours; 40 ℃/h of first phase programming rate, heats up 0.5 hour, is incubated 0.5 hour; 20 ℃/h of second phase programming rate, heats up 1 hour, is incubated 5 hours; 40 ℃/h of three phase programming rates, heats up 0.5 hour, is incubated 8 hours; 40 ℃/h of fourth phase programming rate, heats up 0.5 hour, is incubated 6 hours, and when temperature of charge and heating-up temperature approach, dry end, obtains lyophilizing Radix Rehmanniae extract; With the granulation agent of lyophilizing Radix Rehmanniae extract or tablet or capsule.
Claims (2)
1. lyophilizing Radix Rehmanniae, as the high decoction pieces of bioavailability, is characterized in that: lyophilizing radix rehmanniae bioavailability, higher than Radix Rehmanniae, is more convenient for being processed into Radix Rehmanniae and Radix Rehmanniae Preparata.
According to the lyophilizing Radix Rehmanniae of claim 1 as the high decoction pieces of bioavailability, it is characterized in that: the method for lyophilizing Radix Rehmanniae is: get Radix Rehmanniae, put in freeze dryer, solidification point is controlled between-28～-32 ℃; Reach and control after temperature, open immediately vacuum pump and be evacuated to below drying chamber pressure 50Pa, then start heater switch, promote distillation; The temperature of distillation is controlled at below 40 ℃; The temperature of resolution phase is controlled at below 45 ℃, dry end when temperature of charge and heating-up temperature approach.
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| CN103055017A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Freeze-dried rehmannia for treating diabetes mellitus |
| CN103055024A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Fresh rehmannia powder for treating cancerous fever |
| 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 |
| CN103055019A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Freeze-dried radix rehmanniae recens for treating cerebral thrombus |
| CN103239551A (en) * | 2013-01-16 | 2013-08-14 | 济南康众医药科技开发有限公司 | Freeze-dried radix rehmanniae for preventing and curing obesity |
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- 2014-08-25 CN CN201410418936.6A patent/CN104147225A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055016A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Freeze-dried fresh rehmannia for treating acne |
| CN103055017A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Freeze-dried rehmannia for treating diabetes mellitus |
| CN103055024A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Fresh rehmannia powder for treating cancerous fever |
| 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 |
| CN103055019A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Freeze-dried radix rehmanniae recens for treating cerebral thrombus |
| CN103239551A (en) * | 2013-01-16 | 2013-08-14 | 济南康众医药科技开发有限公司 | Freeze-dried radix rehmanniae for preventing and curing obesity |
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Application publication date: 20141119 |