CN103083596B - Production process of compound herba epimedii immunological enhancement type soluble powder for livestock and poultry - Google Patents
Production process of compound herba epimedii immunological enhancement type soluble powder for livestock and poultry Download PDFInfo
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Abstract
The invention relates to a production process of compound herba epimedii immunological enhancement type soluble powder for livestock and poultry and quality control. The production process of the compound herba epimedii immunological enhancement type soluble powder for the livestock and the poultry comprises the following steps of: drying, sieving, mixing, digesting, concentrating and drying medicinal materials, mixing with auxiliary materials, forming and the like. The quality control comprises the following steps of carrying out establishment of a high performance liquid chromatography gradient eluting program and content measurement on an index component of icariin of herba epimedii carried in PRC (People's Republic of China) Veterinary Pharmacopoeia 2010; and qualitatively surveying appearance uniformity, loss on drying, hygroscopicity and stability. The production process of the compound herba epimedii immunological enhancement type soluble powder for the livestock and the poultry and the quality control provided by the invention have the advantages of high extraction rage of effective components, stable process, high repeatability, low cost and the like. The compound herba epimedii immunological enhancement type soluble powder is uniform color in appearance, small hygroscopicity, optimal mobility, good solubility, high stability, strong reliability of a high performance liquid chromatography content measuring method, less interference, high precision, good repeatability, high accuracy, easiness of operation and the like.
Description
Technical field
The present invention relates to a kind of production technology of animal health-care product, comprising quality control method, be specially the production technology of compound epimedium immunostimulant soluble powder for a kind of poultry.
Background technology
Along with the fast development of intensive culture in China, livestock and poultry development occur becoming increasingly complex, viral disease more and more, also usually with immunosuppressant trend, brought the difficulty of disease prevention, control and treatment, the appearance of particularly immunosuppressant phenomenon, usually cause immuning failure, cause therefrom huge economic loss, make the research and development of immunostimulant become the focus of current veterinary drug industry.
In recent years, there are reports with Chinese herbal medicine, to improve the immunologic function of animal, and some patents have been there are, from the patent of having announced, this class Chinese medicine immunity enhancer is mainly made for powder by pulverizing, or decoction, lixiviate be oral liquid, in poultry, use extremely inconveniently, and be difficult for mix homogeneously.And there is not yet announcement through the patent that Particular craft is made soluble powder.The main not enough performance of issued patents is as follows:
1. some Chinese medicine immunity enhancer is directly that spice after pulverizing medicinal materials is used, and this kind of mode active constituent content is low, and use amount is large, causes poultry to be difficult for searching for food.
2. simple, the technological parameter of processing technique does not have established data, the science shortcoming of EXPERIMENTAL DESIGN, and unstable product quality, is difficult to promote.
3. processing is coarse, and dosage form is single, mostly is powder and powder, and selected evaluation index science is not strong aspect the screening of adjuvant.
4. the product of producing is used inconvenient, mostly is mixed feeding, because consumption in feedstuff is few, is difficult for being mixed evenly, thereby causes the feed intake of animal to be difficult for accurately controlling.
5. aspect the assay of the index components icariin of monarch drug Herba Epimedii, the high performance liquid chromatography of use is equal proportion eluting, but the method is prone to unstability of base line, Interference Peaks in use.
Summary of the invention
Technical problem solved by the invention is to provide the production technology of a kind of poultry with compound epimedium immunostimulant soluble powder, to solve the shortcoming in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
The production technology of compound epimedium immunostimulant soluble powder for poultry, comprise being dried of medical material, pulverize, sieve, lixiviate separation, vacuum concentration, vacuum drying, add adjuvant and be prepared into soluble powder, and the outward appearance uniformity, the loss on drying of product, the investigation of drawing moist, stability, assay, particularly, raw medicinal material Herba Epimedii, Fructus Ligustri Lucidi, the Rhizoma Atractylodis Macrocephalae, Rhizoma Fagopyri Dibotryis, Rhizoma Smilacis Chinensis and Poria are dried to moisture to be 6%, to pulverize, cross pharmacopeia sieve No. 2, be mixed into powder, then add water, the mass ratio of powder and water is 1:8-12; Reflux, extract, after immersion 1h, the time of reflux, extract, is 0.5-1.5h, extracts 1-3 time continuously; The centrifugal 10min of 1000r/min after extracting liquid filtering removal medicinal residues, supernatant becomes after thick extractum in 70 ℃ of vacuum concentration, in 60 ℃ of vacuum dryings, it is dry extract, then add adjuvant, make the gross weight of the raw medicinal material that gross weight equals to drop at first, be pulverized and mixed into soluble powder, with gradient elution program, carry out the assay of icariin, and carry out the outward appearance uniformity, loss on drying, draw the investigation of moist, stability and strong illumination test, the stability of hot and humid accelerated test, long-term stable experiment checking product.
In the present invention, preferably, in lixiviate, add in water process, the mass ratio of described powder and water is 1:10, and described reflux extracting time is 1h, extracts continuously 3 times.
Wherein, the preferred following adjuvant of the present invention matches: described adjuvant is comprised of lactose and soluble starch, and its ratio is 1: 0.5～3.Best, the ratio of described lactose and soluble starch is 1: 1.
Preferred version the most, the described gradient elution program of Determination of Content of Icariin is, take acetonitrile and water as mobile phase, the ratio of front 3min acetonitrile is 24%, the 3～8min, and acetonitrile ratio rises to 50% gradually, 8th～11min, acetonitrile ratio is down to 24%, the 11～15min gradually, and acetonitrile proportions constant is 24%.
beneficial effect
Poultry are used as medicine with decoction with the former side of compound epimedium is clinical, but decoction need face use new system, makes for a long time easy moldy metamorphism, and not portable, mouthfeel is poor, use volume large; Inventory is large directly full presciption medicine material to be pulverized to spice, and abnormal smells from the patient is larger, and poultry are reluctant to search for food, and these have seriously restricted applying of compound epimedium.The present invention is extracted concentrate drying and is become extractum, be prepared into soluble powder with correctives again, both kept decoction to absorb fast, the effective feature such as rapidly, having overcome again decoction takes front interim decoction, is long placed in the mould rotten shortcoming that loses, and can taste masking, poultry are easy to search for food, and cost is lower, can be suitable for large-scale production, also can transport, store, carry, easy to use.
Meanwhile, in extraction process is optimized, we adopt Orthogonal Experiment and Design examination extraction time, add water multiple, extraction time three influence factors' varying level; Take moisture absorption percentage rate, angle of repose, appearance character aspect adjuvant screening as investigating index, in conjunction with the preferred auxiliary material combination of mathematical statistics and proportioning, the problems such as technological parameter is uncertain, quality is unstable have scientifically been solved; What is more important to the index components icariin of product set up higher than existing method accuracy, disturb few Gradient Elution program, and carry out assay, and to the outward appearance uniformity, the loss on drying of product, draw moist, stability and investigate, together carry out quality control, guarantee curative effect.
Accompanying drawing explanation
Fig. 1 is the production technological process of compound epimedium immunostimulant soluble powder for poultry.
Fig. 2 is the HPLC figure of index components icariin in the present invention.
The specific embodiment
Referring to Fig. 1, the production technological process of compound epimedium immunostimulant soluble powder for poultry, the production technology of compound epimedium immunostimulant soluble powder for poultry, comprise the dry of medical material, pulverize, sieve, lixiviate is separated, vacuum concentration, vacuum drying, add adjuvant and be prepared into soluble powder, and the outward appearance uniformity of product, loss on drying, draw moist, stability, the investigation of assay, particularly, by raw medicinal material Herba Epimedii, Fructus Ligustri Lucidi, the Rhizoma Atractylodis Macrocephalae, Rhizoma Fagopyri Dibotryis, it is 6% that Rhizoma Smilacis Chinensis and Poria are dried to moisture, pulverize, cross pharmacopeia sieve No. 2, be mixed into powder, then add water, the mass ratio of powder and water is 1:8-12, reflux, extract, after immersion 1h, the time of reflux, extract, is 0.5-1.5h, extracts 1-3 time continuously, the centrifugal 10min of 1000r/min after extracting liquid filtering removal medicinal residues, supernatant becomes after thick extractum in 70 ℃ of vacuum concentration, in 60 ℃ of vacuum dryings, it is dry extract, then add adjuvant, make the gross weight of the raw medicinal material that gross weight equals to drop at first, be pulverized and mixed into soluble powder, with gradient elution program, carry out the assay of icariin, and carry out the outward appearance uniformity, loss on drying, draw the investigation of moist, stability and strong illumination test, the stability of hot and humid accelerated test, long-term stable experiment checking product.
The present invention will be described in detail for example below.
1. raw materials of traditional Chinese medicinal materials Herba Epimedii, Fructus Ligustri Lucidi, the Rhizoma Atractylodis Macrocephalae, Rhizoma Fagopyri Dibotryis, Rhizoma Smilacis Chinensis and Poria is dry, pulverizing, sieves, 2: 7: 4 in mass ratio: be mixed into powder at 3: 2: 2, add the water of 10 times of medical material weight, put into jacketed pan heating lixiviate; Separation solution and medicinal residues; By solution, through vacuum concentration, be thick extractum, thick extractum is dry extract through vacuum drying.By Orthogonal Experiment and Design examine or check extraction time, add water multiple, extraction time three influence factors' varying level, the optimum extraction process that obtains effective ingredient is the water that medicated powder adds 10 times of weight, soaks 1h, reflux, extract, 1.5h, extracts 3 times continuously.(referring to experiment I)
2. with strengthening mobility, moisture resistance adjuvant lactose, soluble starch, glucose as the object of study of screening, take moisture absorption percentage rate, angle of repose, appearance character as investigating index, first optimize the combination of lactose and soluble starch, with lactose, carry out preferred moulding process from the different proportionings of soluble starch again, the optimum ratio that obtains lactose and soluble starch is 1: 1, has solved the problems such as technological parameter is uncertain, quality is unstable.(referring to experiment II)
3. set up the Gradient Elution program of the index components icariin of monarch drug Herba Epimedii, by setting up quality standard after the aspect checkings such as precision, the response rate, control product quality, and carry out the outward appearance uniformity, loss on drying, draw moist, study on the stability.(seeing experiment III)
4. that under the condition that is 4500Lx ± 500Lx by sample in illumination, places 10d carries out strong illumination test; At 40 ± 2 ℃, relative humidity, it is the hot and humid accelerated test of placing under 75% ± 5% condition 6 months; And the long-term stable experiment of placing 12 months evaluates stability, solved the stability problem of product under the condition of 25 ± 2 ℃ of temperature, relative humidity 60% ± 5%.(seeing experiment IV).
The preferred optimum extraction process of experiment I Orthogonal Experiment and Design
1. factor, level determines
The main pharmacodynamics composition of each raw medicinal material of this product is water solublity, therefore take water as extracting solvent, adopts heating and refluxing extraction method to extract.In conjunction with experience, the main technologic parameters that affects water extraction comprises extraction time, amount of water, extraction time, still to take extraction time, amount of water, extraction time be investigation factor, take each factor extracts the level that usual amounts is each factor, take the paste-forming rate of prescription, the extraction ratio of the index components icariin of monarch drug Herba Epimedii is investigation index, preferably Extraction technique.Factor, level design in Table 1.
Table 1 factor level table
2. test method
According to prescription Chinese crude drug ratio, take medical material, by orthogonal test table L
9(3
4) (summary) test, and calculates the extraction ratio of paste-forming rate and icariin, computing formula is as follows:
Icariin extraction ratio=
Paste-forming rate=
3. test result analysis
Table 2 L
9(3
4) orthogonal experiments
Table 3 paste-forming rate range analysis table
Table 4 paste-forming rate range analysis table
Table 5 icariin extraction ratio range analysis table
Table 6 icariin extraction ratio analysis of variance table
Table look-up and know: F
0.05(2,2)=19
Table 3～table 6 result shows, take paste-forming rate during as index, from intuitive analysis, the factor primary and secondary that affects water extraction effect is sequentially A (extraction time) > C (extraction time) >B (amount of water), optimum level is A3 C3 B3, but the results of analysis of variance shows, in tri-kinds of factors of A, B and C, only have A (extraction time) and C (extraction time) to have significant (P < 0.05) to the impact of Icariin content and yield of extract.Take icariin extraction ratio equally during as index, from intuitive analysis, the factor primary and secondary that affects water extraction effect is sequentially A (extraction time) > C (extraction time) >B (amount of water), optimum level is A3 C3 B3, but the results of analysis of variance shows, in tri-kinds of factors of A, B and C, only have A (extraction time) and C (extraction time) to have significant (P < 0.05) to the impact of Icariin content and yield of extract.
In order to reduce production in enormous quantities cost, final decision extraction process is A3B2C3, adds 10 times of quality of medicinal material water extraction 3 times, each 1.5 h.Empirical tests, process stabilizing, icariin extraction ratio and yield of extract are all higher.
Experiment II is optimized with compound epimedium soluble powder moulding process by poultry
Compound epimedium dry extract yield after extracting is 26%, if while preparing the suitable 1g crude drug of 1g product amount, need to add adjuvant amount to account for 74% of product volume.Intend with strengthening the object of study as screening such as mobility, moisture resistance adjuvant glucose, lactose, soluble starch, take moisture absorption percentage rate, angle of repose, appearance character as investigating index, preferably moulding process.
1. the moisture absorption percentage rate of different auxiliary material and the mensuration of angle of repose
Get dried cream powder appropriate, mix in proportion with adjuvant I (lactose), II (soluble starch), III (glucose), IV (lactose+glucose), V (lactose+soluble starch), VI (glucose+soluble starch) respectively.Get in right amount and measure by the assay method of moisture absorption percentage rate, angle of repose.
The percentile mensuration of 1.1 moisture absorption
Take in proportion a certain amount of compound epimedium dry extract and adjuvant, be dried to constant weight, be placed in bottom and fill in the exsiccator of sodium chloride supersaturated solution, respectively at 6,12,24,48,60h, take quality, calculate moisture absorption percentage rate, the results are shown in Table 7.
The moisture absorption percentage rate mixing of table 7 extract powder and different auxiliary material
Δ is that extract powder is placed the viewed cosmetic variation of 60h;
The mensuration of 1.2 angle of reposes
Adopt fixed funnel method, 3 funnels are connected and be fixed on the At The Height of 1cm on the graph paper of horizontal positioned, carefully the mixture of compound epimedium dry extract and adjuvant is poured into along hopper walls in the funnel of going up most until the dried cream powder cone tip forming on graph paper touches bell mouth, by graph paper, measured the diameter (D) of conical base, calculate angle of repose (tg α=2H/D), repeat 5 times and average, the results are shown in Table 8.
The angle of repose of the mixture of table 8 extract powder and different auxiliary material
His-and-hers watches 7 and table 8 carry out SNK check with SPSS software and obtain table 9.
Table 9 extract powder and data statistic analysis result angle of repose of mixing with different auxiliary material
* there is statistically significant difference (P<0.05).
2. the impact of set adjuvant ratio on dried cream powder hygroscopicity and mobility
Lactose and soluble starch are pressed 2: 1 respectively, and 1: 1,1: 2, take and mix at 1: 3, then get the mixture of appropriate different proportionings, measure as stated above respectively moisture absorption percentage rate and angle of repose, the results are shown in Table 10 and table 11, his-and-hers watches 10 and table 11 carry out SNK check with SPSS software and obtain table 12.
The moisture absorption percentage rate of the different proportioning mixture of table 10
The angle of repose of the different proportioning mixture of table 11
Data statistic analysis result angle of repose of the different proportioning mixture of table 12
* there is statistically significant difference (P<0.05).
From table 10,11,12, the hygroscopicity of mixture declined along with adding of supplementary product consumption, and angle of repose is with corresponding the reducing of increase of consumption; When dried cream powder and adjuvant are fixedly time, the ratio of adjuvant inside is different, there are differences its angle of repose: 2. all have significant difference (P<0.05) with other groups, 1., 3., 4. between there was no significant difference (P > 0.05), consider, when compound epimedium dried cream powder mixes with adjuvant (lactose+soluble starch), lactose and soluble starch ratio are 1: 1 o'clock, hygroscopicity is relatively low, and mobility is better.
Experiment III HPLC measures the content of icariin in compound epimedium immunostimulant soluble powder for poultry
1. instrument and reagent
Shimadzu 2010AHT high performance liquid chromatograph (SIL-20A injector, SPD-20A UV-visible detector, LCSolution work station); Icariin, Nat'l Pharmaceutical & Biological Products Control Institute; Compound epimedium immunostimulant soluble powder for poultry, HuNan NongDa animals Pharmacy Co., Ltd's laboratory provides.Methanol, acetonitrile are chromatographically pure, U.S. world company; All the other are analytical pure, and water is ultra-pure water.
2. method and result
2.1 chromatographic process
Chromatographic column: WATERS Symmetry C18(4.6mm * 150mm, 5 μ m); Mobile phase: water (A)-acetonitrile (B), carries out eluting according to table 13 gradient elution program; Column temperature: 30 ℃; Detect wavelength: 270nm; Flow velocity: 1mL/min; Sample size: 20 μ L; Icariin retention time is 6.2min; Quantitative approach: external standard method.
Table 13 gradient elution program
2.2 content assaying method
2.2.1 it is appropriate that icariin reference substance is got in the preparation of reference substance solution, accurately weighed, add methanol solution and make every 1 mL containing the solution of 0.100mg, with methanol, dilute standardize solution successively again, obtain the serial icariin reference substance solution of 0.080 mg/mL, 0.050 mg/mL, 0.040 mg/mL, 0.030 mg/mL, 0.020 mg/mL, 0.010 mg/mL.
2.2.2 need testing solution preparation precision take this product 1g, precision adds Diluted Alcohol 20ml, supersound process 15min shakes up, and filters, and gets subsequent filtrate, obtains.
2.2.3 the making of standard curve precision is drawn reference substance solution, by the chromatographic condition sample introduction of setting up, analyze, record chromatogram and peak area, take icariin peak area as abscissa, the amount of icariin (μ g) is drawn to obtain icariin standard curve for vertical coordinate, obtains equation of linear regression: y=2 * 10
6x-64594, r=0.9994, Icariin content becomes good linear relation within the scope of 0.204-2.04 μ g with peak area.
2.2.4 the accurate need testing solution of drawing of precision test, repeats sample introduction 6 times by the chromatographic condition of setting up, and the RSD of peak area value is 0.76%.
2.2.5 response rate experiment adds a certain amount of icariin reference substance by measuring precision in the compound epimedium soluble powder of Icariin content, by identical method, processes and measures, and the average recovery rate of icariin is that 99.87%, RSD is 0.94%.
3. sample determination
The accurate test sample sample introduction of drawing, calculates content according to standard curve, the results are shown in Table 14.
Table 14 ten batch sample Determination of Content of Icariin results
Content to icariin in compound epimedium immunostimulant soluble powder is measured, the HPLC assay method of setting up, baseline stability under chromatographic condition used, have fast and convenient, highly sensitive, favorable reproducibility, and in ten batch samples, the content of icariin meets the demands.
The development test of experiment IV sample stability
1. sample source
Three batches of poultry are provided by HuNan NongDa animals Pharmacy Co., Ltd with compound epimedium immunostimulant soluble powder.
2. strong illumination test
By three batches of test samples, be placed under the condition that illumination is 4500Lx ± 500Lx and place 10 days, respectively at sampling in the 5th, 10 days, carry out Determination of Content of Icariin, the results are shown in Table 15.
Table 15 strong illumination result of the test (mgg
-1)
3. hot and humid accelerated test
Three batches of test samples are pressed commercially available back, at 40 ℃ ± 2 ℃, relative humidity, are to place 6 months under 75% ± 5% condition, and respectively at 1 month, 2 months, 3 months and 6 samplings at the end of month, carried out Determination of Content of Icariin, the results are shown in Table 16.
The hot and humid accelerated test result of table 16 (mgg
-1)
4. long-term stable experiment
By three batches of test sample simulation commercially available backs, under the condition of 25 ± 2 ℃ of temperature, relative humidity 60 ± 5%, place 12 months, respectively at sampling in 0 month, 3 months, 6 months, 9 months, 12 months, carry out Determination of Content of Icariin, the results are shown in Table 17.
Table 17 long-term stable experiment result (mgg
-1)
According to above result of the test, the stability of this product is better, and storage condition is: seal, keep in Dark Place.Tentative 12 months of effect duration.
Referring to Fig. 2: the HPLC of index components icariin figure in the present invention, illustrates following examples:
Embodiment mono-, by raw medicinal material Herba Epimedii, Fructus Ligustri Lucidi, the Rhizoma Atractylodis Macrocephalae, Rhizoma Fagopyri Dibotryis, it is 6% that Rhizoma Smilacis Chinensis and Poria are dried to moisture, pulverize, cross pharmacopeia sieve No. 2, press 10 parts of Herba Epimedii, 35 parts of Fructus Ligustri Lucidi, 20 parts of the Rhizoma Atractylodis Macrocephalaes, 15 parts of Rhizoma Fagopyri Dibotryiss, the ratio that 10 parts of Rhizoma Smilacis Chinensiss and Poria are 10 parts is mixed into powder, then the water that adds 8 times of medical material weight, soak 1h, reflux, extract, 0.5h, extract 1 time, the centrifugal 10min of 1000r/min after extracting liquid filtering removal medicinal residues, supernatant at 70 ℃ vacuum concentration to after thick extractum, at 60 ℃, vacuum drying is dry extract, dry extract yield is 18.22%, in gained dry extract, the extraction ratio of icariin is 45.13%.
Embodiment bis-, by raw medicinal material Herba Epimedii, Fructus Ligustri Lucidi, the Rhizoma Atractylodis Macrocephalae, Rhizoma Fagopyri Dibotryis, it is 6% that Rhizoma Smilacis Chinensis and Poria are dried to moisture, pulverize, cross pharmacopeia sieve No. 2, press 10 parts of Herba Epimedii, 35 parts of Fructus Ligustri Lucidi, 20 parts of the Rhizoma Atractylodis Macrocephalaes, 15 parts of Rhizoma Fagopyri Dibotryiss, the ratio that 10 parts of Rhizoma Smilacis Chinensiss and Poria are 10 parts is mixed into powder, then the water that adds 10 times of medical material weight, soak 1h, reflux, extract, 1h, extract 2 times, the centrifugal 10min of 1000r/min after extracting liquid filtering removal medicinal residues, supernatant at 70 ℃ vacuum concentration to after thick extractum, at 60 ℃, vacuum drying is dry extract, dry extract yield is 21.09%, in gained dry extract, the extraction ratio of icariin is 62.54%.
Embodiment tri-, by raw medicinal material Herba Epimedii, Fructus Ligustri Lucidi, the Rhizoma Atractylodis Macrocephalae, Rhizoma Fagopyri Dibotryis, it is 6% that Rhizoma Smilacis Chinensis and Poria are dried to moisture, pulverize, cross pharmacopeia sieve No. 2, press 10 parts of Herba Epimedii, 35 parts of Fructus Ligustri Lucidi, 20 parts of the Rhizoma Atractylodis Macrocephalaes, 15 parts of Rhizoma Fagopyri Dibotryiss, the ratio that 10 parts of Rhizoma Smilacis Chinensiss and Poria are 10 parts is mixed into powder, then the water that adds 12 times of medical material weight, soak 1h, reflux, extract, 1.5h, extract 3 times, the centrifugal 10min of 1000r/min after extracting liquid filtering removal medicinal residues, supernatant at 70 ℃ vacuum concentration to after thick extractum, at 60 ℃, vacuum drying is dry extract, dry extract yield is 26.13%, in gained dry extract, the extraction ratio of icariin is 84.7%.
Embodiment tetra-, by technique described in embodiment tri-, make dry extract, and gained dry extract adds adjuvant to make gross weight equal the to feed intake gross weight of medical material, be pulverized and mixed into soluble powder, adjuvant is comprised of lactose and soluble starch, and its ratio is 1: 0.5 o'clock, and be 36.41 angle of repose.
Embodiment five, by technique described in embodiment tri-, make dry extract, and gained dry extract adds adjuvant to make gross weight equal the to feed intake gross weight of medical material, be pulverized and mixed into soluble powder, adjuvant is comprised of lactose and soluble starch, and its ratio is 1: 2 o'clock, and be 35.66 angle of repose.
Embodiment six, by technique described in embodiment tri-, make dry extract, and gained dry extract adds adjuvant to make gross weight equal the to feed intake gross weight of medical material, be pulverized and mixed into soluble powder, adjuvant is comprised of lactose and soluble starch, and its ratio is 1: 1 o'clock, and be 35.75 angle of repose.
Embodiment seven, by embodiment tri-, make soluble powder with technique described in embodiment six, put in glossy paper, and about 5cm tiles
2, its surface is flattened, at bright place, to observe, color and luster is even, without decorative pattern and mottle.
By above-mentioned technique, make soluble powder, according in bis-appendix of version < < Chinese veterinary pharmacopoeia > > in 2010 " dry weightless mensuration ", 10 batches of compound epimedium soluble powder less loss weight are all no more than 6.0%.
By above-mentioned technique, make soluble powder, get test sample appropriate, put in nessler colorimetric tube, add 2 times of concentration that water 50mL makes clinical use amount, at 25 ℃ ± 2 ℃, spin upside down 10 times, test sample all dissolves, and standing 30min does not have muddiness or precipitation to occur.
By above-mentioned technique, make soluble powder, according to two appendix medicines of the veterinary drug allusion quotation > > of < < People's Republic of China (PRC) version in 2010, drawing moist guideline measures, get one, exsiccator, in bottom, put the culture dish of an interior Sheng saturated aqueous ammonium chloride, put placement 6h in 25 ℃ ± 1 ℃ calorstat and make above moisture stable in exsiccator, humidity is about 89%.Getting external diameter is that 50mm, height are the tool plug glass weighing botle of 15mm, and 105 ℃ of dry 2h put into above-mentioned exsiccator the previous day in testing.Get above-mentioned tool plug glass weighing botle, accurately weighed quality (m
1), test sample is dried to constant weight with proper method in advance, to remove the adsorbed water on medicine powder surface, gets test sample appropriate, puts in weighing botle, accurately weighed quality (m
2).The above-mentioned weighing botle that fills test sample is put in exsiccator, in 25 ℃ ± 1 ℃ insulation, placed 48 hours, take out and claim quality (m
3), and press formula:
Weightening finish percentage rate (%)=
it is 1.8% that wet weightening finish is drawn in calculating, according to the veterinary drug allusion quotation > > of the < < People's Republic of China (PRC) can be defined as slightly draw moist.
By above-mentioned technique, make soluble powder, be 32 ° angle of repose, good fluidity, and critical relative humidity is 65%, and moisture resistance is good, and through hot and humid experiment, in soluble powder, the content of effective ingredient icariin reduces lower than 1%, good stability.
By above-mentioned technique, make soluble powder, be prepared into high performance liquid chromatography test sample and analyze, icariin main peak and impurity peaks separating degree are best, retention time is moderate, peak shape is good, and little to the loss of pump and chromatographic column, is conducive to extend the life-span of chromatographic column, icariin HPLC assay method simultaneously that set up, baseline stability under chromatographic condition used, has fast and convenient, highly sensitive, high repeatability and other advantages, applicable to icariin quantitatively.
Poultry are used as medicine with decoction with the former side of compound epimedium is clinical, but decoction need face use new system, makes for a long time easy moldy metamorphism, and not portable, mouthfeel is poor, use volume large; Inventory is large directly full presciption medicine material to be pulverized to spice, and abnormal smells from the patient is larger, and poultry are reluctant to search for food, and these have seriously restricted applying of compound epimedium, therefore, are necessary that it is carried out to form improvement is beneficial to popularization and application.We thus extracted concentrate drying and become extractum, be prepared into soluble powder with correctives again, both kept decoction to absorb fast, the effective feature such as rapidly, having overcome again decoction takes front interim decoction, is long placed in the mould rotten shortcoming that loses, and can taste masking, poultry are easy to search for food, and cost is lower, can be suitable for large-scale production, also can transport, store, carry, easy to use.Meanwhile, in extraction process is optimized, we adopt Orthogonal Experiment and Design examination extraction time, add water multiple, extraction time three influence factors' varying level; Take moisture absorption percentage rate, angle of repose, appearance character aspect adjuvant screening as investigating index, in conjunction with the preferred auxiliary material combination of mathematical statistics and proportioning, the problems such as technological parameter is uncertain, quality is unstable have scientifically been solved; What is more important to the index components icariin of product set up higher than existing method accuracy, disturb few Gradient Elution program, and carry out assay, and to the outward appearance uniformity, the loss on drying of product, draw moist, stability and investigate, together carry out quality control, guarantee curative effect.
More than show and described ultimate principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and description, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and the claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (5)
1. the production technology of compound epimedium immunostimulant soluble powder for poultry, comprise being dried of medical material, pulverize, sieve, lixiviate separation, vacuum concentration, vacuum drying, add adjuvant and be prepared into soluble powder, and the outward appearance uniformity, the loss on drying of product, the investigation of drawing moist, stability, assay, it is characterized in that, raw medicinal material Herba Epimedii, Fructus Ligustri Lucidi, the Rhizoma Atractylodis Macrocephalae, Rhizoma Fagopyri Dibotryis, Rhizoma Smilacis Chinensis and Poria are dried to moisture to be 6%, to pulverize, cross pharmacopeia sieve No. 2, be mixed into powder, then add water, the mass ratio of powder and water is 1:8-12; Reflux, extract, after immersion 1h, the time of reflux, extract, is 0.5-1.5h, extracts 1-3 time continuously; The centrifugal 10min of 1000r/min after extracting liquid filtering removal medicinal residues, supernatant becomes after thick extractum in 70 ℃ of vacuum concentration, in 60 ℃ of vacuum dryings, it is dry extract, then add adjuvant, make the gross weight of the raw medicinal material that gross weight equals to drop at first, be pulverized and mixed into soluble powder, with gradient elution program, carry out the assay of icariin, and carry out the outward appearance uniformity, loss on drying, draw the investigation of moist, stability and strong illumination test, the stability of hot and humid accelerated test, long-term stable experiment checking product; Described adjuvant is comprised of lactose and soluble starch, and its ratio is 1: 0.5～3.
2. the production technology of compound epimedium immunostimulant soluble powder for poultry according to claim 1, is characterized in that, in lixiviate, add in water process, the mass ratio of described powder and water is 1:10.
3. the production technology of compound epimedium immunostimulant soluble powder for poultry according to claim 1, is characterized in that, described reflux extracting time is 1h, extracts continuously 3 times.
4. the production technology of compound epimedium immunostimulant soluble powder for poultry according to claim 1, is characterized in that, the ratio of described lactose and soluble starch is 1: 1.
5. the production technology of compound epimedium immunostimulant soluble powder for poultry according to claim 1, it is characterized in that, the described gradient elution program of Determination of Content of Icariin is, take acetonitrile and water as mobile phase, and the ratio of front 3min acetonitrile is 24%, 3rd～8min, acetonitrile ratio rises to 50%, the 8～11min gradually, and acetonitrile ratio is down to 24% gradually, 11st～15min, acetonitrile proportions constant is 24%.
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Inventor after: Wu Yong Inventor after: Zhang Mingjun Inventor after: Liu Zikui Inventor after: Liu Xianju Inventor after: Hu Xingping Inventor after: Liu Gaofeng Inventor before: Wu Yong Inventor before: Liu Zikui Inventor before: Liu Xianju Inventor before: Hu Xingping Inventor before: Liu Gaofeng |
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