CN104147057A - Freeze-drying method as method of preparing high-activity penthorum chinense pursh - Google Patents
Freeze-drying method as method of preparing high-activity penthorum chinense pursh Download PDFInfo
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- CN104147057A CN104147057A CN201410418493.0A CN201410418493A CN104147057A CN 104147057 A CN104147057 A CN 104147057A CN 201410418493 A CN201410418493 A CN 201410418493A CN 104147057 A CN104147057 A CN 104147057A
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Abstract
A freeze-drying method as a method for preparing high-activity penthorum chinense pursh. The invention is characterized in that the freeze-drying method is used as the method for preparing penthorum chinense pursh which is high in main effective ingredient content, is high in dissolution rate and is high in bioavailability.
Description
Invention field
The present invention relates to medicine method for making, particularly lyophilization, as the method for preparing high activity Penthorum chinense, belongs to medical technical field.
Background technology
Penthorum chinense is the dry aerial parts of saxifragaceae plant Herba Lysimachiae Clethroids.History is loaded in Ming Dynasty < < Herbal for Relief of Famines > > and now records in 13 > > of < < Ministry of Health of the People's Republic of China ministry standard Traditional Chinese medicine historical preparation, and < < Chinese medicine voluminous dictionary > > and < < Traditional Chinese Medicine in Sichuan will > > are also all on the books.Penthorum chinense is Miao ethnic group's conventional medicament, among the people with its all herbal medicine.Its herb is warm in nature, sweet in the mouth, nontoxic, tool heat clearing away, diuresis elimination of urine, detoxify, invigorate blood circulation, suppressing the hyperactive liver, spleen invigorating, the effects such as yellow cellulitis of dispelling.Cure mainly yellow cellulitis, edema, amenorrhea, metrorrhagia, leukorrhagia, traumatic injury, and various hepatitis, cholecystitis, fatty liver etc.Modern study shows that in Penthorum chinense, total flavones, to the protective effect of hepatic injury tool, can recover liver function, lowers and drinks and the infringement of medicine to liver, suppresses hepatic fibrosis, liver cirrhosis, and to hepatitis A, hepatitis B, chronic active hepatitis tool has significant therapeutic effect.
Penthorum chinense is mainly wild, is mainly distributed in North China, East China, the Central-South and ground such as Shaanxi, Sichuan and Guizhou.Domestication becomes family's kind gradually in recent years, and there is wild and plantation in Shandong.
Summary of the invention
The object of this invention is to provide a kind of method of preparing high activity Penthorum chinense, it is high that Penthorum chinense prepared by the method mainly contains effective component content, and dissolution is high, and bioavailability is good.
The object of the present invention is achieved like this:
Lyophilization, as the method for preparing high activity Penthorum chinense, is characterized in that: it is high that lyophilization mainly contains effective component content as preparation, and dissolution is high, the method for the Penthorum chinense that bioavailability is good.
Lyophilization of the present invention is as the method for preparing high activity Penthorum chinense, it is characterized in that: the method for lyophilizing Penthorum chinense is to be refrigerated to below-10 ℃, be evacuated to below drying chamber pressure 30Pa, subliming by heating, the temperature of distillation should be controlled at below 50 ℃, the temperature of resolution phase is controlled at below 45 ℃, to dry.
So far completed the present invention.The invention provides new purposes or the new object of lyophilizing Penthorum chinense.The application in the Chinese crude drug processing of China of existing lyophilization, object is the activity of preserving to greatest extent effective medicinal components, keeps preferably exterior quality, color, the abnormal smells from the patient of medical material, makes it active suitable with fresh medicine.On the basis of existing technology, those skilled in the art will find apparent that, freeze drying technology is used for to the dry of Penthorum chinense, and the effective ingredient that can preserve to greatest extent Penthorum chinense is active, makes itself and fresh medicine quite active.Lyophilization, for the preparation of Penthorum chinense, makes it mainly contain effective component content high, and dissolution is high, and bioavailability is good, and liver protective effect is good.Those skilled in the art is non-apparent, creative.
Lyophilization, as the method for preparing high activity Penthorum chinense, is the using method that freeze drying technology is new, and its essence does not lie in freeze drying technology itself, and is how to go to use it.It is high that the present invention mainly contains effective component content using lyophilization as preparation, and dissolution is high, and the method for the Penthorum chinense that bioavailability is good is the using method that freeze drying technology is new, possesses novelty.
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 restriction of the present invention.
Fresh Penthorum chinense picks up from Xi Ying town, suburb, Jinan.To, with a collection of fresh Penthorum chinense, process by the following method.
1) dry Penthorum chinense: fresh Penthorum chinense, 80 ℃ of following oven dry.
2) lyophilizing Penthorum chinense: fresh Penthorum chinense, be refrigerated to below-20 ℃, be evacuated to below drying chamber pressure 45Pa, subliming by heating, the temperature of distillation should be controlled at below 40 ℃, and the temperature of resolution phase is controlled at below 45 ℃, to dry.
3) dry Penthorum chinense: fresh Penthorum chinense, be put in shady and cool ventilation place, spread out and dry.
4) fresh Penthorum chinense: without any processing.
One, the content side definite proportion of different dry drying method Penthorum chinense total flavones
1, instrument and reagent
Instrument: the visible spectrophotometer of ultraviolet one; Electronic balance; Control substance of Rutin.
2, detect determining of wavelength
After the colour developing of control substance of Rutin aluminum nitrate, at 500-510nm wavelength place, have absorption maximum, in conjunction with document, test and Selection 500nm is for detecting wavelength.
3, the preparation of reference substance solution
Precision takes the control substance of Rutin 10mg to constant weight at 120 ℃ of drying under reduced pressure, puts in 50mL measuring bottle, adds 70% ethanol 35mL, puts slight fever in water-bath and makes to dissolve, and lets cool, and adds 70% ethanol to scale, shakes up, and obtains (in every mL, containing anhydrous rutin 0.2mg).
4, test sample preparation and assay
Get each 0.1g of Penthorum chinense medical material of above preparation, accurately weighed, put in l00mL volumetric flask, add 70% ethanol 70mL, after jolting, add ethanol to scale, place lh, with dry filter, filter rapidly, precision measures subsequent filtrate 6mL, put in 25mL volumetric flask, add 5% sodium nitrite solution 1mL, mix, place 6min; Add 10% aluminum nitrate solution lmL, shake up, place 6min; Hydro-oxidation sodium test solution 10mL, then add water to scale, shake up, place 15min.
5, side is fixed
According to spectrophotography, at 500nm wavelength place, measure trap, calculate, obtain.The results are shown in Table 1.
The content comparison (n=3) of table 1 total flavones
| Medical material | Dry | Lyophilizing | Dry | Fresh ▲ |
| General flavone content (%) | 5.13 | 9.16 | 5.34 | 9.15 |
▲ fresh Penthorum chinense is in dry product.
By table 1, found out, lyophilizing and fresh Penthorum chinense general flavone content are apparently higher than drying, dry Penthorum chinense.
Two, the dissolution in vitro comparison of lyophilizing Penthorum chinense and fresh Penthorum chinense total flavones
The solution (sodium chloride 2.0g, adds water and dissolve in right amount, adds hydrochloric acid 7ml, is diluted with water to 1000 ml, obtains) of employing pH1.2 is simulated normal person's simulated gastric fluid.Because food is 90-120min at the emptying time of people's gastric, therefore this test is at each point in time sampling of 5-120min.
Get respectively lyophilizing Penthorum chinense and fresh Penthorum chinense, pulverize, cross sieve No. 6, get respectively 6 parts, every part of fresh Penthorum chinense of 0.2g(is in dry product), according to < < Chinese Pharmacopoeia > > Their Dissolution Test in vitro method, measure, the solution 600ml of pH1.2 of take is solvent, rotating speed is 50 r/ min, through 5,10,15,30,45,60,90, during 120 min, get respectively solution 5ml, according to above determination of total flavonoids method, measure, calculate sample at the stripping quantity of different time.The results are shown in Table 2.
Table 2 lyophilizing Penthorum chinense and fresh Penthorum chinense dissolution in vitro comparison (%, n=6)
Table 2 finds out, the dissolution in vitro In Vitro Dissolution of lyophilizing Penthorum chinense total flavones is significantly higher than fresh Penthorum chinense, as well known to those skilled in the art, and medicine is should active constituent content high efficiently, and dissolution rate is high.Above result of the test explanation, lyophilizing Penthorum chinense active constituent content is high, and In Vitro Dissolution rate is high, and then known clinical efficacy is good.
Three, lyophilizing Penthorum chinense and the comparison of fresh Penthorum chinense total flavones bioavailability
The preparation of sample solution: fresh Penthorum chinense is rubbed; Lyophilizing Penthorum chinense was pulverized 40 mesh sieves, and distilled water adds to 4.5 times of amounts (the fresh Penthorum chinense of drying test 4.5g obtains 1g lyophilizing Penthorum chinense).
The preparation of rat blood serum after administration: by 30 of Wistar rats, be divided at random 3 groups, blank group, lyophilizing Penthorum chinense group, fresh Penthorum chinense 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 (0.3 mL/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: accurate serum 2 mL that draw, add methanol 8 mL, vortex vibration 2min, the centrifugal 20min of 3000r/min, gets supernatant, and it is dry that nitrogen dries up instrument, and mobile phase is dissolved, and is settled in 2mL volumetric flask, for ultraviolet spectrophotometry analysis.
The uv-spectrogram contrast of each serum: lyophilizing Penthorum chinense group and the more blank serum group of fresh Penthorum chinense group serum, have more a new chromatographic peak, new chromatographic peak in identical position, illustrates that new chromatographic peak is the characteristic peak of rutin with rutin chromatographic peak.
The peak area that compares rutin in lyophilizing Penthorum chinense group and fresh Penthorum chinense group serum, result, lyophilizing Penthorum chinense group peak area is 1.71 times of fresh Penthorum chinense group serum peak area.Illustrate that lyophilization can prepare the Penthorum chinense that bioavailability is good.
Four, the dry Penthorum chinense liver protective effect comparison of distinct methods
This test adopts CCl
4due to the impact test of Liver Damage in Rats.
The healthy rat of body weight 150-170g, random group, 10 every group, Normal group gives same volume distilled water; Moulding contrast and medicine group are in experiment the 1st, 5 days subcutaneous injection 50% CCl
4vegetable oil rod suspension 5mL/kg gavages respectively water and Penthorum chinense water extract from experiment starts day, and continuous 9 days, 24 hours eye sockets of drug withdrawal were got blood, with reitman-frankel method, survey serum glutamic pyruvic transminase.The results are shown in Table 3.
The dry Penthorum chinense of table 3 distinct methods is to CCl
4the impact of hepatic injury rat blood serum glutamate pyruvate transaminase
| Group | Dosage (g/kg) | Number of animals | Glutamate pyruvate transaminase in serum |
| Normal control | ? | 10 | 19.6±3.4 |
| Moulding pair | ? | 10 | 377.5±120.4 |
| Dry | 3 | 10 | 297.3±123.7 |
| Dry | 3 | 10 | 306.4±125.1 |
| Lyophilizing | 3 | 10 | 235.4±117.5 |
| Fresh ▲ | 3 | 10 | 267.8±116.3 |
▲ fresh Penthorum chinense is in dry product.
The dry Penthorum chinense of distinct methods is to rat CCl
4hepatic injury has protective effect, best with lyophilizing Penthorum chinense action effect.
The specific embodiment
embodiment 1
Get fresh Penthorum chinense, be cut into segment, put in freeze dryer, be refrigerated to below-10 ℃, be evacuated to below drying chamber pressure 30Pa, subliming by heating, the temperature of distillation should be controlled at below 50 ℃, and the temperature of resolution phase is controlled at below 45 ℃, to dry.
embodiment 2
Get fresh Penthorum chinense, be cut into segment, put in freeze dryer, be refrigerated to below-15 ℃, be evacuated to below drying chamber pressure 40Pa, subliming by heating, the temperature of distillation should be controlled at below 45 ℃, and the temperature of resolution phase is controlled at below 45 ℃, to dry.
embodiment 3
Get fresh Penthorum chinense, be cut into segment, put in freeze dryer, be refrigerated to below-28 ℃, be evacuated to below drying chamber pressure 50Pa, subliming by heating, the temperature of distillation should be controlled at below 40 ℃, and the temperature of resolution phase is controlled at below 45 ℃, to dry.
embodiment 4
Get fresh Penthorum chinense, be cut into segment, put in freeze dryer, be refrigerated to below-32 ℃, be evacuated to below drying chamber pressure 45Pa, subliming by heating, the temperature of distillation should be controlled at below 50 ℃, and the temperature of resolution phase is controlled at below 45 ℃, to dry.
Claims (2)
1. lyophilization, as the method for preparing high activity Penthorum chinense, is characterized in that: it is high that lyophilization mainly contains effective component content as preparation, and dissolution is high, the method for the Penthorum chinense that bioavailability is good.
According to the lyophilization of claim 1 as the method for preparing high activity Penthorum chinense, it is characterized in that: the method for lyophilizing Penthorum chinense is to be refrigerated to below-10 ℃, be evacuated to below drying chamber pressure 30Pa, subliming by heating, the temperature of distillation should be controlled at below 50 ℃, the temperature of resolution phase is controlled at below 45 ℃, to dry.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113546032A (en) * | 2020-04-17 | 2021-10-26 | 常州伟博海泰生物科技有限公司 | Allergy-relieving moisture-preserving freeze-dried preparation, instant freeze-dried product, and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829165A (en) * | 2010-05-07 | 2010-09-15 | 张蕊 | Method for preparing alcoholic liver disease medicinal tea by using Penthorum Chinense Pursh |
| CN104147059A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Drying method of penthorum chinense pursh |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101829165A (en) * | 2010-05-07 | 2010-09-15 | 张蕊 | Method for preparing alcoholic liver disease medicinal tea by using Penthorum Chinense Pursh |
| CN104147059A (en) * | 2014-08-25 | 2014-11-19 | 济南康众医药科技开发有限公司 | Drying method of penthorum chinense pursh |
Non-Patent Citations (1)
| Title |
|---|
| 余淑娴等: "真空冷冻干燥技术及其应用", 《食品科技》 * |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113546032A (en) * | 2020-04-17 | 2021-10-26 | 常州伟博海泰生物科技有限公司 | Allergy-relieving moisture-preserving freeze-dried preparation, instant freeze-dried product, and preparation method and application thereof |
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Application publication date: 20141119 |