CN107875184A - A kind of Radix Berberidis extract and preparation method thereof - Google Patents
A kind of Radix Berberidis extract and preparation method thereof Download PDFInfo
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Abstract
The invention provides a kind of preparation method of Radix Berberidis extract, step are as follows：Barberry medicinal powder is taken, by solid-liquid ratio 1:10 20 (g/mL) add the ethanol solution that volume fraction is 45 65%, are flowed back 14 times in 95 DEG C of water-baths, every time 0.5 3h, filter, you can.The Radix Berberidis extract and a kind of Radix Berberidis extract supensoid agent prepared present invention also offers the above method.Content of berberine hydrochloride is high in the Radix Berberidis extract that preparation method of the present invention obtains, and production cost is low；The oral suspensions prepared using Radix Berberidis extract of the present invention, is met standards of pharmacopoeia and stability is good, application prospect is good.
Description
Technical field
The invention belongs to the field of Chinese medicines, and in particular to a kind of Radix Berberidis extract and preparation method thereof.
Background technology
Barberry is that Berberidaceae berberis plan porcupine quill, berberis poiretii, small coptis thorn or spoonleaf barbarry herb etc. belong to plant together
The dry root of thing, the also known as big coptis, shen mahonia root and stem, soulie barberry bark etc. among the people, its main component is Berberine hydrochloride, and major function is
Heat-clearing and damp-drying drug, purging intense heat and detonicating.Modern pharmacological research shows that barberry has extensive antibacterial, antiviral, anti-inflammatory and promotes animal
The effect such as growth and lipid metabolism.In the veterinary clinic application in modern times, barberry is applied to livestock and poultry frequently as feed addictive
Daily ration in, survival rate, control gut flora, the effect for preventing diarrhoea can be improved, while can be used for abdomen caused by Escherichia coli
Rush down, also have been reported that and barberry addition is promoted into lipid metabolism in livestock and poultry diet and improves immunity of organisms, it is seen then that barberry
Good medical prospect is respectively provided with human or animal.
In the production of barberry preparation medicine, the recovery rate of bulk drug Berberine hydrochloride is crucial, is the matter of pharmaceutical preparation
Amount ensures.In existing preparation, from barberry the main boiling of the extracting method of Berberine hydrochloride, acidleach, ultrasound assisted extraction and
The methods of alcohol reflux extracts, but the Berberine hydrochloride recovery rate of various methods is all not fully up to expectations, still needs to further improve.
The content of the invention
In order to solve the above problems, it is an object of the invention to provide a kind of high Radix Berberidis extract extraction side of recovery rate
Method, another object of the present invention is to provide Radix Berberidis extract and a kind of extraction of barberry of a kind of high content of berberine hydrochloride
Thing suspension.
The invention provides a kind of preparation method of Radix Berberidis extract, step are as follows：
Barberry medicinal powder is taken, by solid-liquid ratio 1:It is molten that 10-20 (g/mL) adds the ethanol that volume fraction is 45-65%
Liquid, flowed back 1-4 times in 95 DEG C of water-baths, each 0.5-3h, filtration, you can.
Wherein, the powder is the powder by No. 1 sieve or No. 4 sieves.
Wherein, the solid-liquid ratio is 1:10.
Wherein, the concentration of alcohol is 55%.
Wherein, the number of the backflow is 2 times, each 0.5h.
Wherein, step is as follows：
Barberry medicinal powder is taken, by solid-liquid ratio 1:10 (g/mL) add the ethanol solution that volume fraction is 55%, in 95
Flow back 2 times, each 0.5h, filter in DEG C water-bath, you can.
Present invention also offers Radix Berberidis extract prepared by the above method.
Present invention also offers a kind of suspension containing Radix Berberidis extract, the component of following contents is contained in every 100ml：
Radix Berberidis extract 50ml, disodium ethylene diamine tetraacetate 0.05g, sodium hydrogensulfite 0.1g, sodium benzoate 0.1g, surplus are suspending
Agent and water；
Wherein, the preparation method of the Radix Berberidis extract is：The Radix Berberidis extract described in claim 6 is taken, is concentrated
It is standby to the primary concentrations of 2g/ml.
Wherein, the suspending agent is final concentration of 0.05%-0.15% xanthans；Preferably, the final concentration of xanthans
For 0.10%.
The preparation method of Radix Berberidis extract supensoid agent of the present invention can use conventional supensoid agent technology of preparing, the present invention
A kind of preparation method of above-mentioned Radix Berberidis extract supensoid agent is also provided, step is as follows：The component of each weight proportion is weighed, is mixed
It is even.
The present invention to the factors for influenceing content of berberine hydrochloride by including：Medicinal material granularity, concentration of alcohol, solvent body
After product, return time, reflow's cycle etc. optimize, a kind of high barberry medicinal material extract method of recovery rate, hydrochloric acid have been obtained
Jamaicin recovery rate is up to more than 97.6%；And in the inventive method, it is only necessary to which by pulverizing medicinal materials be coarse powder, solid-liquid ratio is small, second
Determining alcohol is relatively low, low energy consumption, and the cost of refluxing unit is relatively low, is particularly suitable for industrialized production.
The oral suspensions that the present invention is prepared using the Radix Berberidis extract of extraction, meets standards of pharmacopoeia and stability is good,
When disclosure satisfy that oral administration, to the condition of cultivated animals drinking water administration, labor intensity is reduced, is advantageous to the intensive hair of aquaculture
Exhibition, application prospect are good.
Obviously, according to the above of the present invention, according to the ordinary technical knowledge and customary means of this area, do not departing from
Under the premise of the above-mentioned basic fundamental thought of the present invention, the modification, replacement or change of other diversified forms can also be made.
The embodiment of form by the following examples, the above of the present invention is remake further specifically
It is bright.But the scope that this should not be interpreted as to the above-mentioned theme of the present invention is only limitted to following example.It is all to be based on the above of the present invention
The technology realized belongs to the scope of the present invention.
Embodiment
It is described further below with embodiment, but the present invention is not limited to these embodiments.
Experiment reagent and instrument used in the present invention is as follows：
1.1 medicinal material
Barberry, place of production Sichuan, purchased from the side's medicine materical crude slice Co., Ltd of Chengdu thousand, lot number 20101203, content of berberine hydrochloride
10.7mg/g。
1.2 instrument
RE-52CS type Rotary Evaporators, the sub- flourish biochemical instrument instrument factory in Shanghai；ALC-201 type electronic balances, Germany's match are more
Li Si companies；HC-3017 type supercentrifuges, Innovations Zhong Jia branch companies of University of Science and Technology.201 type electric heating air blast thermostatic drying chambers,
Chengdu electric dry oven factory；Agilent-1260 high performance liquid chromatographs, Anjelen Sci. ＆ Tech. Inc.
1.3 reagent
Berberine hydrochloride reference substance, content are calculated as 86.8% by C20H18CINO4, lot number 110713-200911, middle traditional Chinese medicines
Product biological products assay institute.Other reagents are that analysis is pure.
The preparation of 1 Radix Berberidis extract of the present invention of embodiment
Barberry medicinal powder (by No. 1 sieve) 10g is weighed, 55% ethanol 100ml is added, is flowed back in 95 DEG C of water-baths
2 times, each 0.5h, filtration, you can.
The preparation of the Radix Berberidis extract suspension of the present invention of embodiment 2
1st, prescription：
Finally it is settled to 100ml with water (1ml is equivalent to crude drug in whole 1g).
2nd, preparation method is as follows：
Recipe quantity Radix Berberidis extract is taken, sequentially adds the disodium ethylene diamine tetraacetate, sodium hydrogensulfite, benzene first of recipe quantity
Sour sodium, xanthans dissolving, after the completion of be settled to full dose (1ml is equivalent to crude drug in whole 1g).
Beneficial effects of the present invention are illustrated below by way of test example：
The preparation technology of the Radix Berberidis extract of test example 1 investigates
1st, Testing index：
The present invention investigates the extraction process of barberry using the content of berberine hydrochloride of barberry as index, and Berberine hydrochloride contains
Measure and use high-efficient liquid phase technique surely, specific method is as follows：
Chromatographic condition：Using octadecane key and silica gel as filler；With acetonitrile -0.02moL/L potassium dihydrogen phosphates (24:
76) it is mobile phase；Detection wavelength is 265nm, and number of theoretical plate is calculated by Berberine hydrochloride peak should be not less than 4000.
Assay method：Radix Berberidis extract (equivalent to μ g of jamaicin 20) is taken, puts in 50mL volumetric flasks, adds 70% ethanol
To scale, close plug, place 30 minutes, ultrasonic (power 250W, frequency 40kHz) is handled 1 hour, is let cool, and adds 70% ethanol extremely
Scale, shake up, filter, take the μ L of subsequent filtrate 10 inject liquid chromatograph, determine peak area and bring into calibration curve equation calculate contain
Amount.
2nd, the Study on extraction of barberry
2.1 medicinal material granularities
By barberry pulverizing medicinal materials, sieving, the coarse powder by No. 1 sieve, No. 4 fine powders and medicine materical crude slice sieved are taken, are weighed respectively
10g, 55% ethanol 100ml is added, respectively at the 1h filtrations that flowed back in 95 DEG C of water-baths, the ethanol for adding 55% is settled to 100ml,
Detect the content of Berberine hydrochloride in solution and calculate recovery rate.
Recovery rate computational methods are as follows：The content of berberine hydrochloride 10.7mg/g of known medicinal material, extract are concentrated into 1ml phases
When in crude drug in whole 1g, the percentage of Berberine hydrochloride therein and Berberine hydrochloride in medicinal material is recovery rate.
It the results are shown in Table 1.
The influence that the medicinal material granularity of table 1 is extracted to Berberine hydrochloride in barberry
| Granularity | Content of berberine hydrochloride | Recovery rate |
| Medicine materical crude slice | 4.00mg/g | 36.7% |
| Coarse powder | 9.55mg/g | 98.3% |
| Fine powder | 10.68mg/g | 99.9% |
As shown in Table 1, greatly improved by the extraction content of jamaicin after crushing, content and the medicinal material grain of Berberine hydrochloride
Degree is proportionate, but barberry pulverizing medicinal materials dimension fine powder energy consumption is higher, therefore, selects the barberry powder after coarse powder (i.e. complete
Full by No. 1 sieve) as experiment medicinal material.
2.2 process optimization
Precision weighs barberry medicinal powder 10g, takes 15 parts altogether, the ethanol solution of various concentrations is separately added into, in 95
Flow back, filter in DEG C water-bath, the ethanol solution for adding corresponding concentration is settled to original volume, detects content of berberine hydrochloride in solution
And it is scaled medicinal material.The selection result is shown in Table 2.
The influence that 2 different extracting parameters of table extract to Berberine hydrochloride in barberry
| Concentration of alcohol | Return time | Volumes of aqueous ethanol | Reflow's cycle | Content of berberine hydrochloride | Recovery rate | |
| 1 | 45% | 1h | 100ml | 1 | 8.37mg/g | 78.2% |
| 2 | 55% | 1h | 100ml | 1 | 9.68mg/g | 97.5% |
| 3 | 65% | 1h | 100ml | 1 | 8.81mg/g | 82.3% |
| 4 | 75% | 1h | 100ml | 1 | 7.59mg/g | 70.9% |
| 5 | 85% | 1h | 100ml | 1 | 5.75mg/g | 53.7% |
| 6 | 95% | 1h | 100ml | 1 | 4.93mg/g | 46.1% |
| 7 | 55% | 0.5h | 100ml | 1 | 9.76mg/g | 98.2% |
| 8 | 55% | 2h | 100ml | 1 | 9.34mg/g | 87.3% |
| 9 | 55% | 3h | 100ml | 1 | 91.7mg/g | 85.7% |
| 10 | 55% | 0.5h | 50ml | 1 | 7.62mg/g | 71.2% |
| 11 | 55% | 0.5h | 150ml | 1 | 10.26mg/g | 98.9% |
| 12 | 55% | 0.5h | 200ml | 1 | 10.67mg/g | 99.7% |
| 13 | 55% | 0.5h | 100ml | 2 | 9.60mg/g | 99.7% |
| 14 | 55% | 0.5h | 100ml | 3 | 9.61mg/g | 99.9% |
| 15 | 55% | 0.5h | 100ml | 4 | 9.65mg/g | 98.2% |
As shown in Table 2, when concentration of alcohol is 55%-65%, the recovery rate of Berberine hydrochloride is higher, with carrying for concentration of alcohol
Height, recovery rate decline；Other volumes of aqueous ethanol, return time, reflow's cycle have an impact to the recovery rate of Berberine hydrochloride.
Wherein, concentration of alcohol 55%-65%, solid-liquid ratio 1:10-20 (g/mL), flows back 1-4 times in 95 DEG C of water-baths,
Each 0.5-3h, filtration, can effectively extract Berberine hydrochloride, consider recovery rate and extraction cost, select following extract
Technique：Concentration of alcohol is 55%, solid-liquid ratio 1:10 (g/mL), flow back 2 times, each 0.5h, filter in 95 DEG C of water-baths.
2.3 extraction checking tests
Precision weighs barberry medicinal powder 10g, 4 parts, is separately added into 55% ethanol 100ml, is returned in 95 DEG C of water-baths
Stream 2 times, each 0.5h, filtration, the ethanol for being separately added into 55% are settled to 100ml, detect the content of Berberine hydrochloride, checking is most
The extraction process selected eventually.
It the results are shown in Table 3.
Table 3 extracts checking test
As shown in Table 3, the standard deviation of Berberine hydrochloride recovery rate is 0.85, the coefficient of variation 0.96%, far smaller than
2%, illustrate that difference is not notable, experiment precision is high, reproducible.
The preparation technology of the Radix Berberidis extract suspension of test example 2 investigates
Because barberry medicinal material is extracted with 55% ethanol, there is precipitation to generate after concentration, therefore be prepared as being suspended
Agent.
1st, the inspection target of supensoid agent
(1) content
Detected with reference to the assay method of extract.
(2) sedimentation volume ratio
Apparatus plug graduated cylinder measures test sample 50ml, close plug, firmly shakes 1min, writes down the beginning height H0 of suspended matter, quiet
Put 3 hours, write down the final height H of suspended matter, be calculated as follows：
Sedimentation volume ratio=H/H0, sedimentation volume ratio are not less than 0.90.
(3) syringeability
Test sample is taken, is used after shaking with No. 9 needle aspirates, volume aspirated is no less than 2ml in 1 minute.
(4) it is dispersed
With reference to the centrifugation standard of emulsion, by test sample to be shaken after 4000r/min rotating speed centrifugation 15min, should easily disperse.
2nd, the Study on Preparation of suspension
It is standby that Radix Berberidis extract is concentrated into the primary concentrations of 2g/ml, add antioxidant, complexing of metal ion agent and
After preservative, the influence of suspending agent is investigated.
(1) species of suspending agent
Selection conventional oral suspending agent such as sodium carboxymethylcellulose, gelatin, Arabic gum, xanthans, agar, obtain as
Lower prescription：
Suspending agent is added by the usual amounts of various suspending agents
Finally it is settled to 100ml with water (1ml is equivalent to crude drug in whole 1g).
5 kinds of Radix Berberidis extract supensoid agents are prepared by above-mentioned prescription, testing result is shown in Table 4.
The suspension effect expedition of 4 various supensoid agents of table
| Suspending agent kind | Addition | Syringeability | Sedimentation volume ratio | Content | Dispersiveness |
| Sodium carboxymethylcellulose | 0.5% | 4.5ml | 98% | 9.26mg/ml | It is easily scattered |
| Arabic gum | 0.5% | 3.6ml | 100% | 9.21mg/ml | It is easily scattered |
| Xanthans | 0.1% | 4.8ml | 100% | 9.20mg/ml | It is easily scattered |
| Gelatin | 0.5% | 3.2ml | 100% | 9.15mg/ml | It is easily scattered |
| Agar | 0.1% | 3.5ml | 100% | 9.32mg/ml | It is easily scattered |
As shown in Table 7, the Radix Berberidis extract suspension that prepared by various suspending agents meets standard, therefore, this 5 kinds of suspendings
Agent can be used.
Because this product is oral formulations, drinking-water or spice after generally diluting during use, therefore tackle the suspension after dilution
Situation is investigated.It the results are shown in Table 5.
Suspension effect expedition after the various suspension dilution agents of table 5 (sedimentation time occurs in record)
| Suspending agent kind | 25 times | 50 times | 100 times | 200 times | 400 times | 800 times |
| Sodium carboxymethylcellulose | 48h | 24h | 12h | 3h | 0 | 0 |
| Arabic gum | 48h | 48h | 48h | 48h | 24h | 12h |
| Xanthans | 48h | 48h | 48h | 48h | 48h | 48h |
| Gelatin | 48h | 48h | 48h | 48h | 48h | 24h |
| Agar | 48h | 48h | 48h | 48h | 48h | 24h |
As shown in Table 5, the supensoid agent prepared with Arabic gum, gelatin, xanthans, agar can continue to mix after being diluted with water
It is outstanding, but the suspension effect of xanthans can continue 48 hours (respectively at 3h, 6h, 12h, 24h, 48h), and gelatin and agar take second place,
The sodium carboxymethylcellulose duration is most short, it is therefore preferable that being used as suspending agent using xanthans.
(2) dosage of suspending agent
Dosage of the xanthans in supensoid agent is investigated, obtains following prescription：
Finally it is settled to 100ml (1ml is equivalent to crude drug in whole 1g).
6 parts of samples are prepared using above prescription, testing result is shown in Table 6-7.
The suspension effect expedition of 6 various supensoid agents of table
| Addition | Syringeability | Sedimentation volume ratio | Content | Dispersiveness |
| 0.05% | 5.4ml | 100% | 9.18mg/ml | It is easily scattered |
| 0.10% | 4.7ml | 100% | 9.23mg/ml | It is easily scattered |
| 0.15% | 3.2ml | 100% | 9.34mg/ml | It is easily scattered |
| 0.20% | 1.8ml | 100% | 9.25mg/ml | It is easily scattered |
| 0.25% | 1.0ml | 100% | 9.24mg/ml | It is not easy to disperse |
| 0.30% | 0.6ml | 100% | 9.16mg/ml | It is not easy to disperse |
As shown in Table 6, after xanthans addition 0.2%, syringeability reduces, and does not meet《Chinese veterinary pharmacopoeia》To the rule of supensoid agent
Fixed, therefore, the broiler diets of xanthans are 0.05%-0.15%.
Be suspended situation after the dilution of investigation xanthans difference addition, the results are shown in Table 7.
Suspension effect expedition after the various suspension dilution agents of table 7 (sedimentation time occurs in record)
| Addition | 25 times | 50 times | 100 times | 200 times | 400 times | 800 times |
| 0.05% | 48h | 48h | 48h | 48h | 48h | 24h |
| 0.10% | 48h | 48h | 48h | 48h | 48h | 48h |
| 0.15% | 48h | 48h | 48h | 48h | 48h | 48h |
As shown in Table 7, during xanthans addition 0.10-0.15%, suspension effect can be stablized and continue 48 hours, therefore, comprehensive
Consider suspension effect, therefore, the addition for selecting xanthans is 0.10%.
To sum up, the present invention has obtained a kind of high barberry medicinal material extract method of recovery rate by optimizing extracting parameter；And
And the inventive method energy consumption is low, operating cost is low, is particularly suitable for industrialized production.The present invention utilizes the Radix Berberidis extract extracted
The oral suspensions of preparation, meets standards of pharmacopoeia and stability is good, and application prospect is good.
Claims (10)
- A kind of 1. preparation method of Radix Berberidis extract, it is characterised in that：Step is as follows：Barberry medicinal powder is taken, by solid-liquid ratio 1:10-20 (g/mL) adds the ethanol solution that volume fraction is 45-65%, in Flowed back 1-4 times in 95 DEG C of water-baths, each 0.5-3h, filtration, you can.
- 2. preparation method according to claim 1, it is characterised in that：The powder is the powder by No. 1 sieve or No. 4 sieves End.
- 3. preparation method according to claim 1, it is characterised in that：The solid-liquid ratio is 1:10.
- 4. preparation method according to claim 1, it is characterised in that：The concentration of alcohol is 55%.
- 5. preparation method according to claim 1, it is characterised in that：The number of the backflow is 2 times, each 0.5h.
- 6. preparation method according to claim 1, it is characterised in that：Step is as follows：Barberry medicinal powder is taken, by solid-liquid ratio 1:10 (g/mL) add the ethanol solution that volume fraction is 55%, in 95 DEG C of water Flow back 2 times, each 0.5h, filter in bath, you can.
- 7. Radix Berberidis extract prepared by claim 1~6 any one methods described.
- A kind of 8. suspension containing Radix Berberidis extract, it is characterised in that：Contain the component of following contents in per 100ml：Radix Berberidis extract 50ml, disodium ethylene diamine tetraacetate 0.05g, sulfurous acid Hydrogen sodium 0.1g, sodium benzoate 0.1g, surplus are suspending agent and water；Wherein, the preparation method of the Radix Berberidis extract is：The Radix Berberidis extract described in claim 6 is taken, is concentrated into 2g/ The primary concentrations of ml, it is standby.
- 9. suspension according to claim 8, it is characterised in that：The suspending agent is final concentration of 0.05%-0.15% Xanthans；Preferably, final concentration of the 0.10% of xanthans.
- 10. the preparation method of the suspension of claim 8 or 9, it is characterised in that：Step is as follows：Weigh the component of each weight proportion, mixing.
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| CN108371672A (en) * | 2018-05-09 | 2018-08-07 | 四川师范大学 | Purposes of the golden flower barberries extract in preparing anti-oxidant class drug |
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| CN107050023A (en) * | 2017-01-13 | 2017-08-18 | 北京顺慈医药科技有限公司 | A kind of preparation of Berberine hydrochloride and the formulation method for covering adverse drug taste |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107050023A (en) * | 2017-01-13 | 2017-08-18 | 北京顺慈医药科技有限公司 | A kind of preparation of Berberine hydrochloride and the formulation method for covering adverse drug taste |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108371672A (en) * | 2018-05-09 | 2018-08-07 | 四川师范大学 | Purposes of the golden flower barberries extract in preparing anti-oxidant class drug |
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Application publication date: 20180406 |