CN104180617A - Freeze-drying method of rehmannia glutinosa - Google Patents
Freeze-drying method of rehmannia glutinosa Download PDFInfo
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- CN104180617A CN104180617A CN201410418764.2A CN201410418764A CN104180617A CN 104180617 A CN104180617 A CN 104180617A CN 201410418764 A CN201410418764 A CN 201410418764A CN 104180617 A CN104180617 A CN 104180617A
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Abstract
The invention relates to a freeze-drying method of rehmannia glutinosa. The freeze-drying method is characterized in that the fresh rehmannia glutinosa is selected to be freeze-dried till completion of sublimation. The prepared rehmannia glutinosa in the freeze-drying method is high in content of an active ingredient of catalpol, high in bioavailability and low in energy consumption, products are not easy to smash, decoction pieces are easy to keep in shape during storage and transport, and quality of the products is stable.
Description
Invention field
The present invention relates to medicine method for making, particularly the freeze drying process of a kind of glutinous rehmannia, belongs to medical technical field.
Background technology
Fresh medicine application is characteristic and the special shape of middle medical drugs, and its feature has: cool nature medicine fresh goods is compared with the cooler inclined to one side profit of dry product; Pungent fragrance medicine fresh goods is high compared with the rich power of dry product; It is rapid-action that the fresh medicine concoction power of moisturizing is better than dry product.Because fresh medicine contains abundant natural smell and the pure strong drug action of its taste of juice, having directly promotes the production of body fluid increases the effect of liquid, and the title that is always subject to ancient Chinese medicine doctor is high.
Existing fresh medicine preservation technique has nature preservative, Sha Zangfa, Sha Zhifa, Storage in cold bank method, plastic sheeting fresh-keeping method etc.But because existing fresh medicine preservation technique falls behind, storage tolerance, is not easy to transportation, and seasonal strong, so that fresh medicine supply is out of stock for a long time, and most fresh medicines all replace with dry product.Clinical research is verified, much Chinese medicine, and dry product can not substitute fresh goods in some cases.
Freeze-drying is widely applied for fresh medicine new fresh keeping technique and processing method China, in the Chinese medicines such as glutinous rehmannia, ginseng, American Ginseng, Cordyceps sinensis, Chinese yam, matrimony vine, pilose antler, all appears in the newspapers.Freeze drying technology can be preserved the activity of effective medicinal components to greatest extent, keeps preferably exterior quality, color, the smell of medicinal material, makes fresh and alive plant or animal drug keep the effect of fresh medicine.But freeze-drying medicinal material quality loose gently crisp, product is frangible, is difficult for keeping medicine materical crude slice shape.
Summary of the invention
The freeze drying process that the object of this invention is to provide a kind of glutinous rehmannia, the freeze-drying rehmannia catalpol content of preparation is high, and energy consumption is low, and medicine materical crude slice keeping quality is good.
Object of the present invention is achieved through the following technical solutions:
A freeze drying process for glutinous rehmannia, is characterized in that: get fresh rehmannia root, put in freeze dryer, solidification point is controlled between-28～-32 ℃; Reach and control after temperature, be evacuated to immediately below drying chamber pressure 50Pa, heating sublimation then, the temperature of distillation is controlled at below 40 ℃, and distillation finishes, and takes out, and obtains.
The freeze drying process of a kind of glutinous rehmannia of the present invention, is characterized in that: a kind of judgement of distillation in finishing by the following method 1. serviceability temperature Sensor monitoring temperature of charge judge whether the ice in material all distils; 2. condenser temperature drops to the state before distillation; 3. the pressure drop of freeze drying box is to the pressure that approaches freezer unit.
So far completed the present invention, freeze dried fresh ground active ingredient catalpol content prepared by the present invention is high, and bioavilability is high, and energy consumption is low, and product is non-friable, and storage, transportation easily keep medicine materical crude slice shape, constant product quality.
The freeze-drying of existing freeze drying technology is vacuum freeze drying by name entirely, refers to medicinal material is freezed at low temperatures, then under vacuum condition, distils, and removes ice crystal, after distillation finishes, carries out adsorption stripping and dry again, and remove portion is in conjunction with the drying means of water.The steps such as freezing dry process mainly can be divided into primary drying (distillation), redrying (desorb).The difference of the present invention and existing freeze drying technology is no longer to carry out redrying after distillation finishes, and energy consumption is low.
Below by test example, further illustrate usefulness of the present invention.
One, prepare sample
The fresh rehmannia root of being gathered in same plot simultaneously, process respectively by the following method:
1) fresh rehmannia root: new fresh rehmannia root soil buries, plastic bag sealing moisturizing;
2) radix rehmanniae recen: get fresh rehmannia root, be cut into sheet, 60 ℃ are slowly cured to eighty per cant dry;
3) freeze-drying glutinous rehmannia of the present invention, gets fresh rehmannia root, is cut into sheet, puts in freeze dryer, and solidification point is controlled between-28～-32 ℃; Reach and control after temperature, be evacuated to immediately below drying chamber pressure 50Pa, heating sublimation then, the temperature of distillation is controlled at below 40 ℃, and distillation finishes, and takes out, and obtains.
4) freeze-drying glutinous rehmannia, gets fresh rehmannia root, is cut into sheet, puts in freeze dryer, and solidification point is controlled between-28～-32 ℃; Reach and control after temperature, be evacuated to immediately below drying chamber pressure 50Pa, heating sublimation then, the temperature of distillation is controlled at below 40 ℃, and resolution temperature is controlled at below 45 ℃, to dry, takes out, and obtains.
Two, catalpol content comparison in different dry drying method glutinous rehmannia
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: fresh rehmannia root is rubbed, and dried rehamnnia root was pulverized 40 mesh sieves, the fresh rehmannia root 2.5g(drying of accurately weighed rubbing test 5g fresh rehmannia root obtains 1g freeze-drying glutinous rehmannia respectively), freeze-drying radix rehmanniae 0.5g, add methyl alcohol 25mL, weigh, ultrasonic processing 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.
Catalpol content in table 1 different dry drying method glutinous rehmannia
| ? | Catalpol content (%) |
| Fresh rehmannia root | 6.18 |
| Radix rehmanniae recen | 0.73 |
| Freeze-drying glutinous rehmannia of the present invention | 5.66 |
| Freeze-drying glutinous rehmannia | 5.67 |
Table 1 result is known, and freeze-drying glutinous rehmannia of the present invention and freeze-drying rehmannia catalpol content are basic identical, all apparently higher than radix rehmanniae recen.
Three, different dry drying method glutinous rehmannia friability comparison
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 samples 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 2.
Table 2 different dry drying method glutinous rehmannia friability
| ? | Shatter (%) | Less loss amount (%) |
| Radix rehmanniae recen | Nothing | 0.54 |
| Freeze-drying glutinous rehmannia of the present invention | Nothing | 0.89 |
| Freeze-drying glutinous rehmannia | 60 | 5.93 |
Table 2 result is known, and freeze-drying glutinous rehmannia friability of the present invention is good, and antivibration wear resistant ability is strong, and product is non-friable, and storage, transportation easily keep medicine materical crude slice shape, constant product quality.
Four, different dry drying method glutinous rehmannia bioavilability comparison
1, 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.
2, 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.
3, the preparation of sample solution: fresh rehmannia root is rubbed; Radix rehmanniae recen, freeze-drying glutinous rehmannia of the present invention and freeze-drying glutinous rehmannia, pulverized 40 mesh sieves, and distilled water adds to (drying test 5g fresh rehmannia root obtains 1g freeze-drying glutinous rehmannia) of amount in 5 times.
4, the preparation of rat blood serum after administration: by 30 of Wistar rats, be divided at random 5 groups, blank group, fresh rehmannia root group, radix rehmanniae recen group, freeze-drying glutinous rehmannia group of the present invention and freeze-drying glutinous rehmannia 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% chloraldurate (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.
5, the processing of serum: the accurate serum 2mL that draws, add methyl alcohol 8mL, vortex vibration 2min, the centrifugal 20min of 3000r/min, gets supernatant, and it is dry that nitrogen dries up instrument, mobile phase dissolves, be settled in 2mL volumetric flask, 0.45 μ m filtering with microporous membrane, for efficient liquid phase chromatographic analysis.
6, result: the high efficiency liquid phase collection of illustrative plates contrast of each serum: fresh rehmannia root group, radix rehmanniae recen group, freeze-drying glutinous rehmannia group of the present invention and the more blank serum group of freeze-drying glutinous rehmannia 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.
Comparison peak area, result, freeze-drying glutinous rehmannia group ≈ freeze-drying glutinous rehmannia group > fresh rehmannia root group > radix rehmanniae recen group of the present invention.Freeze-drying glutinous rehmannia group peak area is 1.28 times of fresh rehmannia root group peak area, and freeze-drying glutinous rehmannia group of the present invention is 1.27 times of fresh rehmannia root group peak area, and radix rehmanniae recen group is 0.78 times of fresh rehmannia root group peak area.Illustrate that freeze-drying glutinous rehmannia of the present invention is suitable with freeze-drying glutinous rehmannia bioavilability, be better than fresh rehmannia root and radix rehmanniae recen, radix rehmanniae recen is minimum.
Four, freeze-drying glutinous rehmannia quality stability of the present invention is investigated
Freeze-drying glutinous rehmannia of the present invention, aluminum-plastic composite membrane packs.Use accelerated stability test method, 40 ℃ ± 2 ℃ of temperature, under the experimental condition of relative humidity 75% ± 5%, (experimental condition control: electro-heating standing-temperature cultivator, NaCl saturated solution) placed, respectively at 1,2,3, measure test sample catalpol content June.
4, result of the test: result of the test is in Table 3.
Table 3 freeze-drying glutinous rehmannia of the present invention quality stability is investigated result
| ? | 0 month | 1 month | 2 months | 3 months | 6 months |
| Catalpol content (%) | 5.66 | 5.65 | 5.65 | 5.67 | 5.66 |
Table 3 is found out, freeze-drying glutinous rehmannia steady quality of the present invention.
The specific embodiment
A freeze drying process for glutinous rehmannia, is characterized in that: get fresh rehmannia root, put in freeze dryer, solidification point is controlled between-28～-32 ℃; Reach and control after temperature, be evacuated to immediately below drying chamber pressure 50Pa, heating sublimation then, the temperature of distillation is controlled at below 40 ℃, and distillation finishes, and takes out, and obtains.
The freeze drying process of a kind of glutinous rehmannia of the present invention, is characterized in that: a kind of judgement of distillation in finishing by the following method 1. serviceability temperature Sensor monitoring temperature of charge judge whether the ice in material all distils; 2. condenser temperature drops to the state before distillation; 3. the pressure drop of freeze drying box is to the pressure that approaches freezer unit.
embodiment 1
Get fresh rehmannia root, put in freeze dryer, solidification point is controlled at-28 ℃; Reach and control after temperature, open immediately vavuum 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 ℃, when ice all distils, finishes.
embodiment 2
Get fresh rehmannia root, put in freeze dryer, solidification point is controlled at-32 ℃; Reach and control after temperature, open immediately vavuum 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 ℃; During state before condenser temperature drops to distillation, finish.
embodiment 3
Get fresh rehmannia root, put in freeze dryer, solidification point is controlled at-30 ℃; Reach and control after temperature, open immediately vavuum 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 ℃; When the pressure drop of freeze drying box to approach freezer unit pressure time finish.
embodiment 4
Get fresh rehmannia root, put in freeze dryer, solidification point is controlled at-29 ℃; Reach and control after temperature, open immediately vavuum 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 ℃, to distillation end, takes out, and obtains.
Claims (2)
1. a freeze drying process for glutinous rehmannia, is characterized in that: get fresh rehmannia root, put in freeze dryer, solidification point is controlled between-28～-32 ℃; Reach and control after temperature, be evacuated to immediately below drying chamber pressure 50Pa, heating sublimation then, the temperature of distillation is controlled at below 40 ℃, and distillation finishes, and takes out, and obtains.
2. according to the freeze drying process of a kind of glutinous rehmannia of claim 1, it is characterized in that: a kind of judgement of distillation in finishing by the following method 1. serviceability temperature Sensor monitoring temperature of charge judge whether the ice in material all distils; 2. condenser temperature drops to the state before distillation; 3. the pressure drop of freeze drying box is to the pressure that approaches freezer unit.
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Citations (5)
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| CN101228896A (en) * | 2007-10-23 | 2008-07-30 | 江南大学 | Method of combining freeze-dry and vacuum microwave drying to preparing fruits, vegetables and aquatic leisure food |
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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 |
| 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
- 2014-08-25 CN CN201410418764.2A patent/CN104180617A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101228896A (en) * | 2007-10-23 | 2008-07-30 | 江南大学 | Method of combining freeze-dry and vacuum microwave drying to preparing fruits, vegetables and aquatic leisure food |
| CN103055015A (en) * | 2013-01-10 | 2013-04-24 | 济南康众医药科技开发有限公司 | Radix rehmanniae recens for treating habitual constipation |
| 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 |
| 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 |
| 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: 20141203 |