CN103083596A - 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 that a kind of poultry are used compound epimedium immunostimulant soluble powder.
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, improve more existing reports of immunologic function of animal with Chinese herbal medicine, and some patents have appearred, from the patent of having announced, this class Chinese medicine immunity enhancer mainly is made for powder by pulverizing, or decoction, lixiviate be oral liquid, uses extremely inconveniently in poultry, and is 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 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. process coarsely, 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 uses inconvenient, mostly is mixed feeding, because consumption in feedstuff is few, is difficult for mixing 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 the 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 the above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
The poultry production technology of compound epimedium immunostimulant soluble powder, comprise medical material drying, 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, draw investigation moist, stable, 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 the pharmacopeia sieve No. 2, be mixed into powder, then add entry, 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 is after 70 ℃ of vacuum concentration become thick extractum, be dry extract in 60 ℃ of vacuum dryings, 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, carry out the assay of icariin with the gradient elution program, and carry out the outward appearance uniformity, loss on drying, draw moist, stable investigation and strong illumination test, the stability of hot and humid accelerated test, long-term stable experiment checking product.
In the present invention, preferably, add in the water process in lixiviate, 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 is that 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 the acetonitrile ratio rises to 50% gradually, the 8th～11min, the acetonitrile ratio is down to 24%, the 11～15min gradually, and the 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 and use new system, make for a long time easy moldy metamorphism, and not portable, mouthfeel is poor, uses volume large; Inventory is large directly the full presciption medicine material to be pulverized 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 extracts concentrate drying with it and becomes extractum, be prepared into soluble powder with correctives again, both kept decoction to absorb the characteristics such as fast, that produce effects is rapid, having overcome again decoction takes front interim decoction, is long placed in the mould rotten shortcoming that loses, but and 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.
Simultaneously, in extraction process was optimized, we adopted 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 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 aspect the adjuvant screening; What is more important is set up the Gradient Elution program higher than existing method accuracy, that interference is lacked to the index components icariin of product, 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.
Description of drawings
Fig. 1 is the production technological process that poultry are used compound epimedium immunostimulant soluble powder.
Fig. 2 is the HPLC figure of index components icariin in the present invention.
The specific embodiment
referring to Fig. 1, the poultry production technological process of compound epimedium immunostimulant soluble powder, the poultry production technology of compound epimedium immunostimulant soluble powder, the drying that comprises medical material, pulverize, sieve, lixiviate separates, 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, with the 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 the pharmacopeia sieve No. 2, be mixed into powder, then add entry, 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 is after 70 ℃ of vacuum concentration become thick extractum, be dry extract in 60 ℃ of vacuum dryings, 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, carry out the assay of icariin with the gradient elution program, and carry out the outward appearance uniformity, loss on drying, draw moist, stable investigation 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 for the 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, sieve, 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; Be thick extractum with solution through vacuum concentration, thick extractum is dry extract through vacuum drying.By Orthogonal Experiment and Design examine or check extraction time, add the water multiple, extraction time three influence factors' varying level, the optimum extraction process that gets 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 the 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, come preferred moulding process with lactose from the different proportionings of soluble starch again, the optimum ratio that gets lactose and soluble starch is 1: 1, has solved the problems such as technological parameter is uncertain, quality is unstable.(referring to the 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 checking of the aspects 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 the experiment III)
4. with sample in illumination be place 10d under the condition of 4500Lx ± 500Lx carry out the strong illumination test; Be to place the hot and humid accelerated test of 6 months under 75% ± 5% condition at 40 ± 2 ℃, relative humidity; And the long-term stable experiment evaluation of placing 12 months under the condition of 25 ± 2 ℃ of temperature, relative humidity 60% ± 5% is stable, has solved the stability problem of product.(seeing the 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, adopt the 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 take extraction time, amount of water, extraction time as the investigation factor, extract usual amounts as the level of each factor take each factor, take the extraction ratio of the index components icariin of paste-forming rate, the monarch drug Herba Epimedii of prescription as investigating index, preferred Extraction technique.Factor, level design see Table 1.
Table 1 factor level table
2. test method
Take medical material according to prescription Chinese crude drug ratio, press 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:
The 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, during take paste-forming rate as index, from intuitive analysis as seen, the factor primary and secondary that affects the water extraction effect sequentially is 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 three kinds of factors of A, B and C, to only have A (extraction time) and C (extraction time) on the impact of Icariin content and yield of extract, significant (P＜0.05) to be arranged.During equally take the icariin extraction ratio as index, from intuitive analysis as seen, the factor primary and secondary that affects the water extraction effect sequentially is 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 three kinds of factors of A, B and C, only have A (extraction time) and C (extraction time) on the impact of Icariin content and yield of extract, significant (P＜0.05) to be arranged.
In order to reduce the production in enormous quantities cost, the final decision extraction process is A3B2C3, namely 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.
The experiment II is optimized with compound epimedium soluble powder moulding process by poultry
Compound epimedium dry extract yield after extracting is 26%, if when preparing the suitable 1g crude drug of 1g product amount, need to add the 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, preferred moulding process.
1. the moisture absorption percentage rate of different auxiliary material and the mensuration of angle of repose
Get dried cream powder appropriate, respectively with adjuvant I (lactose), II (soluble starch), III (glucose), IV (lactose+glucose), V (lactose+soluble starch), VI (glucose+soluble starch) mixing in proportion.Get in right amount and measure by the assay method of moisture absorption percentage rate, angle of repose.
1.1 the percentile mensuration of moisture absorption
Take in proportion a certain amount of compound epimedium dry extract and adjuvant, be dried to constant weight, be placed in the bottom and fill in the exsiccator of sodium chloride supersaturated solution, take quality respectively at 6,12,24,48,60h, calculate the moisture absorption percentage rate, the results are shown in Table 7.
The moisture absorption percentage rate that mixes of table 7 extract powder and different auxiliary material
Δ is that extract powder is placed the viewed cosmetic variation of 60h;
1.2 the mensuration of angle of repose
Adopt the fixed funnel method, 3 funnels are connected and be fixed in 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 that forms on graph paper touches bell mouth, measured the diameter (D) of conical base by graph paper, calculate (tg α=2H/D) angle of repose, 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 the 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
* has statistically significant difference (P＜0.05).
2. the impact of set adjuvant ratio on dried cream powder hygroscopicity and mobility
Lactose and soluble starch were pressed 2: 1 respectively, and 1: 1,1: 2, take at 1: 3 and mixing, 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 the 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
* has statistically significant difference (P＜0.05).
By table 10,11,12 as can be known, the hygroscopicity of mixture descended along with adding of supplementary product consumption, and reduce with the increase of consumption is corresponding angle of repose; When dried cream powder and adjuvant fixedly the time, the ratio of adjuvant inside is different, there are differences its angle of repose: 2. with other groups, significant difference (P＜0.05) is arranged all, 1., 3., 4. between there was no significant difference (P＞0.05), consider, when mixing, lactose and soluble starch ratio are 1: 1 o'clock to the compound epimedium dried cream powder with adjuvant (lactose+soluble starch), hygroscopicity is relatively low, and mobility is better.
Experiment III HPLC measures the content that poultry are used icariin in compound epimedium immunostimulant soluble powder
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; Poultry compound epimedium immunostimulant soluble powder, 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), carry out eluting according to table 13 gradient elution program; Column temperature: 30 ℃; Detect wavelength: 270nm; Flow velocity: 1mL/min; Sample size: 20 μ L; The 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 the icariin reference substance is got in the preparation of reference substance solution, accurately weighed, add methanol solution and make the solution that every 1 mL contains 0.100mg, dilute standardize solution with methanol 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 the preparation precision take this product 1g, precision adds Diluted Alcohol 20ml, supersound process 15min shakes up, and filters, and gets subsequent filtrate, and get final product.
2.2.3 the accurate reference substance solution of drawing of the making of standard curve, analyze by the chromatographic condition sample introduction of setting up, record chromatogram and peak area, take the icariin peak area as abscissa, the amount of icariin (μ g) is drawn to get the icariin standard curve for vertical coordinate, obtains equation of linear regression: y=2 * 10
6X-64594, r=0.9994, namely Icariin content becomes the good linear relation with peak area in 0.204-2.04 μ g scopes.
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, the RSD of peak area value is 0.76%.
2.2.5 the response rate is tested, and in the compound epimedium soluble powder that will measure Icariin content, precision adds a certain amount of icariin reference substance, processes and measures by identical method, 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
With three batches of test samples, be placed under the condition that illumination is 4500Lx ± 500Lx and placed 10 days, respectively at sampling in the 5th, 10 day, 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, are to place 6 months under 75% ± 5% condition at 40 ℃ ± 2 ℃, relative humidity, respectively at 1 month, and 2 months, 3 months and take a sample 6 the end of month, carry 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
With three batches of test sample simulation commercially available backs, placed 12 months under the condition of 25 ± 2 ℃ of temperature, relative humidity 60 ± 5%, 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 one, with the 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 the 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 in 70 ℃ of lower vacuum concentration to the thick extractum, 60 ℃ of lower vacuum dryings are dry extract, the dry extract yield is 18.22%, in the gained dry extract, the extraction ratio of icariin is 45.13%.
embodiment two, with the 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 the 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 in 70 ℃ of lower vacuum concentration to the thick extractum, 60 ℃ of lower vacuum dryings are dry extract, the dry extract yield is 21.09%, in the gained dry extract, the extraction ratio of icariin is 62.54%.
embodiment three, with the 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 the 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 in 70 ℃ of lower vacuum concentration to the thick extractum, 60 ℃ of lower vacuum dryings are dry extract, the dry extract yield is 26.13%, in the gained dry extract, the extraction ratio of icariin is 84.7%.
Embodiment four, make dry extract by the described technique of embodiment three, and the 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, make dry extract by the described technique of embodiment three, and the 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, make dry extract by the described technique of embodiment three, and the 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, make soluble powder by embodiment three with the described technique of embodiment six, put on glossy paper, and approximately 5cm tiles
2, its surface is flattened, to observe at bright place, color and luster is even, without decorative pattern and mottle.
Make soluble powder by above-mentioned technique, according in two appendix of version " Chinese veterinary pharmacopoeia " in 2010 " dry weightless mensuration ", 10 batches of compound epimedium soluble powder less loss weight all are no more than 6.0%.
Make soluble powder by above-mentioned technique, get test sample appropriate, in the Zhi Nashi color comparison tube, add 2 times of concentration that water 50mL makes clinical use amount, spin upside down 10 times at 25 ℃ ± 2 ℃, test sample all dissolves, and standing 30min does not have muddiness or precipitation to occur.
Make soluble powder by above-mentioned technique, drawing moist guideline according to two appendix medicines of " People's Republic of China's veterinary drug allusion quotation " version in 2010 measures, get one, exsiccator, put the culture dish of an interior Sheng saturated aqueous ammonium chloride in the bottom, put in 25 ℃ ± 1 ℃ calorstat and make moisture stable in exsiccator more than placement 6h, 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 medicine powder surface sorption water, 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, placed 48 hours in 25 ℃ ± 1 ℃ insulation, take out title quality (m
3), and by formula:
Weightening finish percentage rate (%)=
It is 1.8% that wet weightening finish is drawn in calculating, according to " People's Republic of China's veterinary drug allusion quotation " can be defined as slightly draw moist.
Make soluble powder by above-mentioned technique, 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.
Make soluble powder by above-mentioned technique, be prepared into the 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, the icariin HPLC assay method of setting up simultaneously, 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 and use new system, make for a long time easy moldy metamorphism, and not portable, mouthfeel is poor, uses volume large; Inventory is large directly the full presciption medicine material to be pulverized 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 form improvement is beneficial to popularization and application.We thus it extracted concentrate drying become extractum, be prepared into soluble powder with correctives again, both kept decoction to absorb the characteristics such as fast, that produce effects is rapid, having overcome again decoction takes front interim decoction, is long placed in the mould rotten shortcoming that loses, but and 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.Simultaneously, in extraction process was optimized, we adopted 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 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 aspect the adjuvant screening; What is more important is set up the Gradient Elution program higher than existing method accuracy, that interference is lacked to the index components icariin of product, 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.
Above demonstration 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 describes in above-described embodiment and description 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 (6)
1. poultry are with the production technology of compound epimedium immunostimulant soluble powder, comprise medical material drying, 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, draw investigation moist, stable, 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 the pharmacopeia sieve No. 2, be mixed into powder, then add entry, 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 is after 70 ℃ of vacuum concentration become thick extractum, be dry extract in 60 ℃ of vacuum dryings, 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, carry out the assay of icariin with the gradient elution program, and carry out the outward appearance uniformity, loss on drying, draw moist, stable investigation and strong illumination test, the stability of hot and humid accelerated test, long-term stable experiment checking product.
2. poultry according to claim 1 with the production technology of compound epimedium immunostimulant soluble powder, is characterized in that, add in the water process in lixiviate, the mass ratio of described powder and water is 1:10.
3. poultry according to claim 1 with the production technology of compound epimedium immunostimulant soluble powder, is characterized in that, described reflux extracting time is 1h, extracts continuously 3 times.
4. poultry according to claim 1 with the production technology of compound epimedium immunostimulant soluble powder, is characterized in that, described adjuvant is comprised of lactose and soluble starch, and its ratio is 1: 0.5～3.
5. poultry according to claim 4 with the production technology of compound epimedium immunostimulant soluble powder, is characterized in that, the ratio of described lactose and soluble starch is 1: 1.
6. poultry according to claim 1 are with the production technology of compound epimedium immunostimulant soluble powder, it is characterized in that, 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 3rd～8min, the acetonitrile ratio rises to 50%, the 8～11min gradually, and the acetonitrile ratio is down to 24% gradually, the 11st～15min, the acetonitrile proportions constant is 24%.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104820049A (en) * | 2015-03-17 | 2015-08-05 | 中山市中智药业集团有限公司 | Fingerprint spectrum common mode construction and quality detection method for epimedium herb wall-breaking decoction pieces |
| CN111505164A (en) * | 2020-05-19 | 2020-08-07 | 华中农业大学 | Method for determining biological BCS solubility of common oral antibacterial drugs for pigs |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422500A (en) * | 2008-12-12 | 2009-05-06 | 湖南农业大学 | Immunoenhancement regulator of pig blue-ear disease vaccine and use thereof |
-
2013
- 2013-02-20 CN CN201310054119.2A patent/CN103083596B/en active Active
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422500A (en) * | 2008-12-12 | 2009-05-06 | 湖南农业大学 | Immunoenhancement regulator of pig blue-ear disease vaccine and use thereof |
Non-Patent Citations (6)
| Title |
|---|
| 崔保安等: "有机硒和某些中草药对鸡免疫功能的影响", 《畜牧与兽医》, vol. 35, no. 10, 31 October 2003 (2003-10-31) * |
| 张声生等: "中医补益药增强机体免疫力在AIDS中的运用简报", 《江西中医学院学报》, vol. 4, no. 01, 31 December 1992 (1992-12-31) * |
| 汪德刚等: "《兽药中药学》", 29 February 2008, article "多能性", pages: 46 * |
| 石达友等: "中药提取物对鸡免疫器官发育和新城疫抗体水平的影响", 《中兽医学杂志》, vol. 4, no. 02, 31 December 2004 (2004-12-31) * |
| 郑艳等: "《中药资源教育》", 31 July 2010, article "中药饲料添加剂开发", pages: 173-174 * |
| 陈群: "植物多糖免疫调节作用和抗肿瘤活性", 《安庆师范学院学报(自然科学版)》, vol. 7, no. 01, 28 February 2001 (2001-02-28) * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104820049A (en) * | 2015-03-17 | 2015-08-05 | 中山市中智药业集团有限公司 | Fingerprint spectrum common mode construction and quality detection method for epimedium herb wall-breaking decoction pieces |
| CN104820049B (en) * | 2015-03-17 | 2016-06-08 | 中山市中智药业集团有限公司 | The finger printing common pattern of Herba Epimedii breaking cellular wall decoction pieces builds and quality determining method |
| CN111505164A (en) * | 2020-05-19 | 2020-08-07 | 华中农业大学 | Method for determining biological BCS solubility of common oral antibacterial drugs for pigs |
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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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