CN104940147A - Tilmicosin premix and preparation method thereof - Google Patents
Tilmicosin premix and preparation method thereof Download PDFInfo
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- CN104940147A CN104940147A CN201510366423.XA CN201510366423A CN104940147A CN 104940147 A CN104940147 A CN 104940147A CN 201510366423 A CN201510366423 A CN 201510366423A CN 104940147 A CN104940147 A CN 104940147A
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- Prior art keywords
- tilmicosin
- mixing agent
- antioxidant
- starch
- add
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- JTSDBFGMPLKDCD-XVFHVFLVSA-N tilmicosin Chemical compound O([C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CCN1C[C@H](C)C[C@H](C)C1)CO[C@H]1[C@@H]([C@H](OC)[C@H](O)[C@@H](C)O1)OC)CC)[C@@H]1O[C@H](C)[C@@H](O)[C@H](N(C)C)[C@H]1O JTSDBFGMPLKDCD-XVFHVFLVSA-N 0.000 title claims abstract description 103
- 229960000223 tilmicosin Drugs 0.000 title claims abstract description 99
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- 239000003963 antioxidant agent Substances 0.000 claims abstract description 16
- 230000003078 antioxidant effect Effects 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims description 58
- 238000002156 mixing Methods 0.000 claims description 58
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 claims description 40
- 229920002472 Starch Polymers 0.000 claims description 34
- 239000008107 starch Substances 0.000 claims description 34
- 235000019698 starch Nutrition 0.000 claims description 34
- 229920001817 Agar Polymers 0.000 claims description 21
- 239000008272 agar Substances 0.000 claims description 21
- 235000010265 sodium sulphite Nutrition 0.000 claims description 20
- 239000011230 binding agent Substances 0.000 claims description 17
- 238000003756 stirring Methods 0.000 claims description 14
- 239000003085 diluting agent Substances 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 239000002002 slurry Substances 0.000 claims description 9
- 239000000203 mixture Substances 0.000 claims description 8
- 239000008187 granular material Substances 0.000 claims description 7
- 239000012467 final product Substances 0.000 claims description 6
- 239000007779 soft material Substances 0.000 claims description 6
- 239000004375 Dextrin Substances 0.000 claims description 5
- 229920001353 Dextrin Polymers 0.000 claims description 5
- GUBGYTABKSRVRQ-QKKXKWKRSA-N Lactose Natural products OC[C@H]1O[C@@H](O[C@H]2[C@H](O)[C@@H](O)C(O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@H]1O GUBGYTABKSRVRQ-QKKXKWKRSA-N 0.000 claims description 5
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 5
- 229930006000 Sucrose Natural products 0.000 claims description 5
- 235000019425 dextrin Nutrition 0.000 claims description 5
- 239000008101 lactose Substances 0.000 claims description 5
- HRZFUMHJMZEROT-UHFFFAOYSA-L sodium disulfite Chemical compound [Na+].[Na+].[O-]S(=O)S([O-])(=O)=O HRZFUMHJMZEROT-UHFFFAOYSA-L 0.000 claims description 5
- 235000010262 sodium metabisulphite Nutrition 0.000 claims description 5
- 239000005720 sucrose Substances 0.000 claims description 5
- 238000004090 dissolution Methods 0.000 claims description 4
- 238000001035 drying Methods 0.000 claims description 4
- GUBGYTABKSRVRQ-XLOQQCSPSA-N Alpha-Lactose Chemical compound O[C@@H]1[C@@H](O)[C@@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@H](O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-XLOQQCSPSA-N 0.000 claims description 3
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 2
- 235000011152 sodium sulphate Nutrition 0.000 claims description 2
- 239000003814 drug Substances 0.000 abstract description 26
- 229940079593 drug Drugs 0.000 abstract description 14
- 241001465754 Metazoa Species 0.000 abstract description 9
- 239000000463 material Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 244000144977 poultry Species 0.000 abstract description 5
- 238000010521 absorption reaction Methods 0.000 abstract description 2
- 244000144972 livestock Species 0.000 abstract description 2
- 239000000853 adhesive Substances 0.000 abstract 1
- 230000001070 adhesive effect Effects 0.000 abstract 1
- 230000037406 food intake Effects 0.000 abstract 1
- 239000002994 raw material Substances 0.000 abstract 1
- 230000000153 supplemental effect Effects 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 22
- 241000282898 Sus scrofa Species 0.000 description 9
- 238000010438 heat treatment Methods 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 238000000034 method Methods 0.000 description 7
- 239000000843 powder Substances 0.000 description 6
- 239000000273 veterinary drug Substances 0.000 description 6
- NESIVXZOSKKUDP-ARVJLQODSA-N (4r,5s,6s,7r,9r,11e,13e,15r,16r)-6-[(2r,3r,4s,5s,6r)-4-(dimethylamino)-3,5-dihydroxy-6-methyloxan-2-yl]oxy-7-[2-[(3s,5r)-3,5-dimethylpiperidin-1-yl]ethyl]-16-ethyl-4-hydroxy-15-[[(2r,3r,4r,5r,6r)-5-hydroxy-3,4-dimethoxy-6-methyloxan-2-yl]oxymethyl]-5,9,13 Chemical compound OP(O)(O)=O.O([C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CCN1C[C@H](C)C[C@H](C)C1)CO[C@H]1[C@@H]([C@H](OC)[C@H](O)[C@@H](C)O1)OC)CC)[C@@H]1O[C@H](C)[C@@H](O)[C@H](N(C)C)[C@H]1O NESIVXZOSKKUDP-ARVJLQODSA-N 0.000 description 5
- 241000202934 Mycoplasma pneumoniae Species 0.000 description 5
- 230000001133 acceleration Effects 0.000 description 5
- 238000013112 stability test Methods 0.000 description 5
- 208000024891 symptom Diseases 0.000 description 5
- 230000001225 therapeutic effect Effects 0.000 description 5
- 229960000757 tilmicosin phosphate Drugs 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 238000005286 illumination Methods 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 206010011224 Cough Diseases 0.000 description 3
- 206010013786 Dry skin Diseases 0.000 description 3
- 208000007271 Substance Withdrawal Syndrome Diseases 0.000 description 3
- 208000006673 asthma Diseases 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 230000000857 drug effect Effects 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 241000204031 Mycoplasma Species 0.000 description 2
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- 238000010171 animal model Methods 0.000 description 2
- JQVDAXLFBXTEQA-UHFFFAOYSA-N dibutylamine Chemical compound CCCCNCCCC JQVDAXLFBXTEQA-UHFFFAOYSA-N 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 238000002955 isolation Methods 0.000 description 2
- 239000002932 luster Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- ZMOUALJOEYJPSZ-BDMZYGHZSA-N (4r,5s,6s,7r,9r,11e,13e,15s,16r)-6-[(2r,3r,4s,5s,6r)-4-(dimethylamino)-3,5-dihydroxy-6-methyloxan-2-yl]oxy-7-[2-[(3s,5r)-3,5-dimethylpiperidin-1-yl]ethyl]-16-ethyl-4-hydroxy-15-[(2s,3r,4r,5r,6r)-5-hydroxy-3,4-dimethoxy-6-methyloxan-2-yl]oxy-5,9,13-trimeth Chemical compound O([C@@H]1[C@@H](C)[C@H](O)CC(=O)O[C@@H]([C@H](/C=C(\C)/C=C/C(=O)[C@H](C)C[C@@H]1CCN1C[C@H](C)C[C@H](C)C1)O[C@H]1[C@@H]([C@H](OC)[C@H](O)[C@@H](C)O1)OC)CC)[C@@H]1O[C@H](C)[C@@H](O)[C@H](N(C)C)[C@H]1O ZMOUALJOEYJPSZ-BDMZYGHZSA-N 0.000 description 1
- 241000894006 Bacteria Species 0.000 description 1
- 241000283690 Bos taurus Species 0.000 description 1
- 241000283707 Capra Species 0.000 description 1
- 208000035473 Communicable disease Diseases 0.000 description 1
- FEWJPZIEWOKRBE-JCYAYHJZSA-N Dextrotartaric acid Chemical compound OC(=O)[C@H](O)[C@@H](O)C(O)=O FEWJPZIEWOKRBE-JCYAYHJZSA-N 0.000 description 1
- 241000192125 Firmicutes Species 0.000 description 1
- 241000287828 Gallus gallus Species 0.000 description 1
- 241000605008 Spirillum Species 0.000 description 1
- 241000282887 Suidae Species 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 description 1
- 206010047700 Vomiting Diseases 0.000 description 1
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 208000022531 anorexia Diseases 0.000 description 1
- 230000000844 anti-bacterial effect Effects 0.000 description 1
- 230000000843 anti-fungal effect Effects 0.000 description 1
- 229940121375 antifungal agent Drugs 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 210000003850 cellular structure Anatomy 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 206010061428 decreased appetite Diseases 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 230000037213 diet Effects 0.000 description 1
- 235000005911 diet Nutrition 0.000 description 1
- 230000008034 disappearance Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 230000009977 dual effect Effects 0.000 description 1
- 238000002592 echocardiography Methods 0.000 description 1
- 230000003203 everyday effect Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000000796 flavoring agent Substances 0.000 description 1
- 235000019634 flavors Nutrition 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 238000009472 formulation Methods 0.000 description 1
- 235000011389 fruit/vegetable juice Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 208000015181 infectious disease Diseases 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000000968 intestinal effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000003120 macrolide antibiotic agent Substances 0.000 description 1
- 229920000609 methyl cellulose Polymers 0.000 description 1
- 239000001923 methylcellulose Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000005070 sampling Methods 0.000 description 1
- 239000012047 saturated solution Substances 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 235000010288 sodium nitrite Nutrition 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Landscapes
- Pharmaceuticals Containing Other Organic And Inorganic Compounds (AREA)
Abstract
The invention relates to the field of medicines for livestock and poultry, and particularly provides a tilmicosin premix and a preparation method thereof. The tilmicosin premix is prepared from the following raw materials in percentage by mass: 5%-50% of tilmicosin, 0.5%-20% of an adhesive and 0.05%-2% of an antioxidant. According to the tilmicosin premix provided by the invention, the medicine odor of the tilmicosin is covered; ingestion of animals is not affected; the tilmicosin premix is wide in raw and supplemental material source, low in cost, and relatively high in absorption speed in an animal body; the bioavailability is greatly improved, so that the dosage of the tilmicosin is reduced; the medicine effect is improved; and the cost is also reduced.
Description
Technical field
The present invention relates to poultry with medicament field, specifically, relate to a kind of tilmicosin pre-mixing agent and preparation method thereof.
Background technology
Tilmicosin (Timicosin) is the special antibiotic of a kind of semi-synthetic Macrolide poultry, there is very strong antibacterial activity, has a broad antifungal spectrum, all has inhibitory action to all gram positive bacterias and part gram negative bacteria, Mycoplasma, spirillum, mycoplasma etc.This medicine successively to go through clinical application in countries such as Australia, Brazil, France, Malaysia, Italy, Spain, the U.S., is used for the treatment of the infectious disease of the animals such as goat, milch cow, pig, chicken.The existing approved tilmicosin class medicine of China is used for the clinical treatment of livestock and poultry animal, at present mainly through administration for oral administration, but tilmicosin bitter in the mouth, the anorexia of poultry can be caused in administration process, the ill symptomses such as nausea and vomiting, cause the failure of administration.In order to solve above-mentioned Problems existing, the object of the invention is to provide a kind of with low cost, and production technology is simple, and can meet the tilmicosin pre-mixing agent of national standard.
Summary of the invention
In order to realize the object of the invention, the invention provides a kind of tilmicosin pre-mixing agent and preparation method thereof.
A kind of tilmicosin pre-mixing agent, by percentage to the quality, containing following component: tilmicosin 5%-50%, binding agent 0.5%-20%, antioxidant 0.05%-2%; Preferably containing following component: tilmicosin 8%-30%, binding agent 1%-10%, antioxidant 0.1%-1.5%; More preferably containing following component: tilmicosin 10%-20%, binding agent 2%-4%, antioxidant 0.5%-1%.
Further, described tilmicosin is the mixture of one or more in tilmicosin, tilmicosin salt.Described tilmicosin salt is the mixture of one or more in tilmicosin phosphate, tartaric acid tilmicosin etc.
Further, described binding agent is the mixture of one or more in agar, starch slurry, cellulose derivative; Preferred described binding agent is agar.When the present invention finds to select agar as binding agent, its cohesive and water solublity are better than starch slurry, solve granule better and hold breakable problem.
Further, described antioxidant is the mixture of one or more in sodium sulfate, sodium sulfite, sodium sulfite, sodium pyrosulfite; Be preferably sodium sulfite.Preferred sodium sulfite well solves as antioxidant the stable problem that tilmicosin tires.
Described tilmicosin pre-mixing agent also comprises diluent, and described diluent is preferably one or more in starch, dextrin, lactose, sucrose.Described diluent is preferably starch; Safe, inexpensive, wide material sources.
Particularly, described tilmicosin pre-mixing agent also comprises diluent starch, gathers to total amount to 100% with described diluent starch.
The present invention also provides a kind of preparation method of above-mentioned tilmicosin pre-mixing agent, and described method comprises the steps:
1) get suitable quantity of water and dissolve antioxidant, for subsequent use; General water consumption is 50-60 times of antioxidant quality;
2) to step 1) obtained by solution in add binding agent, stir, for subsequent use; Suitable quantity of water can be added again if desired; When selecting agar to be binding agent, needing heating that agar is dissolved, being generally heated to 60-80 DEG C, after stirring, being generally cooled to 50-60 DEG C;
3) to step 2) obtained by solution in add tilmicosin and stir, add diluent, granulate after making soft material, dry (general baking temperature 60-80 DEG C), sieve (No. 2 can be selected to sieve or No. 4 sieves), to obtain final product.
Beneficial effect of the present invention:
Tilmicosin pre-mixing agent provided by the present invention, masks the drug flavor of tilmicosin, does not affect searching for food of animal; Tilmicosin pre-mixing agent of the present invention meets the quality standard of pharmacopeia; Pre-mixing agent production equipment of the present invention is simple, does not use in special production equipment; This pre-invention pre-mixing agent is with low cost, supplementary material wide material sources; And pre-mixing agent of the present invention is because dispersion in solids, has larger surface area, absorbs faster in animal body.Described tilmicosin pre-mixing agent major auxiliary burden is starch, dextrin, lactose, sucrose, wide material sources, low price.Described binding agent can form cellular structure, increases the surface area that medicine contacts with intestinal juice, accelerates the absorption of medicine, improves curative effect of medication.In addition, because the effect of active component tilmicosin is not fully exerted, bioavailability is greatly improved, thus reduces the consumption of tilmicosin, not only increases drug effect, also a saving cost.
Detailed description of the invention
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Embodiment 1
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin 10kg, and agar powder 2kg, sodium sulfite 1kg; Surplus is starch.
Embodiment 2
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin 20kg, and agar powder 2kg, sodium sulfite 0.5kg; Surplus is starch.
Embodiment 3
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin 10kg, and agar powder 2kg, starch slurry 2kg, sodium sulfite 1kg; Surplus is starch.
Embodiment 4
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin 30kg, and starch slurry 10kg, sodium pyrosulfite 1.5kg; Surplus is starch.
Embodiment 5
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin phosphate 5kg, and methylcellulose 0.5kg, sodium sulfite 0.05kg; Surplus is starch and lactose, and starch and lactose mass ratio are 200: 1.
Embodiment 6
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin 30kg, and agar powder 5kg, starch slurry 5kg, sodium pyrosulfite 1kg; Surplus is starch and sucrose, and starch and sucrose mass ratio are 100: 1.
Embodiment 7
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin 10kg, and agar powder 2kg, sodium pyrosulfite 0.5kg; Surplus is starch and dextrin, and starch and dextrin mass ratio are 10: 1.
Embodiment 8
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin phosphate 15kg, and starch slurry 4kg, sodium sulfite 1kg; Surplus is starch.
Embodiment 9
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin phosphate 50kg, and starch slurry 20kg, sodium sulfite 2kg; Surplus is starch.
Embodiment 10
The present embodiment provides a kind of tilmicosin pre-mixing agent, in 100kg, containing following component: tilmicosin phosphate 20kg, and agar powder 4kg, sodium sulfite 1kg; Surplus is starch.
Embodiment 11
The present embodiment provides a kind of preparation method of tilmicosin pre-mixing agent, and the formula of described tilmicosin pre-mixing agent is with embodiment 1, and described method specifically comprises the steps:
1) 55 times of water dissolution sodium sulfite of sodium sulfite quality are got, for subsequent use;
2) to step 1) obtained by solution in add agar, be heated to 70 DEG C and agar dissolved, stir, then be cooled to 55 DEG C, for subsequent use;
3) to step 2) obtained by solution in add tilmicosin and stir, add starch, make in the rearmounted granulator of soft material and granulate, in 80 DEG C of dryings, through No. 2 sieved sieves, to obtain final product.
Embodiment 12
The present embodiment provides a kind of preparation method of tilmicosin pre-mixing agent, and the formula of described tilmicosin pre-mixing agent is with embodiment 2, and described method specifically comprises the steps:
1) 60 times of water dissolution sodium sulfite of sodium sulfite quality are got, for subsequent use;
2) to step 1) obtained by solution in add agar, be heated to 60 DEG C and agar dissolved, stir, then be cooled to 50 DEG C, for subsequent use;
3) to step 2) obtained by solution in add tilmicosin and stir, add starch, make in the rearmounted granulator of soft material and granulate, in 80 DEG C of dryings, through No. 2 sieved sieves, to obtain final product.
Embodiment 13
The present embodiment provides a kind of preparation method of tilmicosin pre-mixing agent, and the formula of described tilmicosin pre-mixing agent is with embodiment 3, and described method specifically comprises the steps:
1) 50 times of water dissolution sodium sulfite of sodium sulfite quality are got, for subsequent use;
2) to step 1) obtained by solution in add agar and starch slurry, be heated to 80 DEG C and agar dissolved, stir, then be cooled to 60 DEG C, for subsequent use;
3) to step 2) obtained by solution in add tilmicosin and stir, add starch, make in the rearmounted granulator of soft material and granulate, in 80 DEG C of dryings, through No. 4 sieved sieves, to obtain final product.
The effect of experimental example 1 tilmicosin pre-mixing agent clinical trial treatment mycoplasma pneumoniae of swine
1, test objective
In order to verify the drug effect of tilmicosin pre-mixing agent provided by the invention, the tilmicosin pre-mixing agent that this test obtains by the embodiment of the present invention 2 and control formulation are respectively to mycoplasma pneumoniae of swine therapeutic test.Test data gathers according to testing program in batches.
2, test material
2.1 use medicine
2.1.1 trial drug 1: the tilmicosin pre-mixing agent that embodiment 2 is obtained.
2.1.2 control drug 2: certain company produce 20% tilmicosin pre-mixing agent (product batch number: 20140306, it consists of tilmicosin 20%, starch is 80%.
2.2 experimental animal and grouping
2.2.1 pig farm, Xiangtan County market pig 982, about 95 ages in days, wherein has 120 to occur cough and asthma.Select at random wherein 20 as blank group, all the other 100 pigs are divided into 2 groups (trial drug group, control drug groups) at random, often organize 50.
3, test method
3.1 trial drug treated animals are labeled as A group, and feedstuff per ton adds 1 kilogram of trial drug 1.
3.2 control drug treated animals are labeled as B group, add 1 kilogram of control drug 2 by feedstuff per ton.
3.3 blank group echos are C group, only give chow diet, do not add any medicine.
The equal continuous use of above-mentioned experimental animal 7 days, observes 5 days again after medication, observes clinical symptoms and death condition every day, cut open inspection to animals died of illness.Calculate the effective percentage of each test group, cure rate, Relapse rate situation.
3.4 criterion
3.4.1 effective: clinical symptom relief (cough and asthma or alleviate, spirit take a turn for the better, growth take a turn for the better etc.).
3.4.2 cure: clinical symptom disappearance (cough and asthma stop, and spirit takes a turn for the better, growth recovery is normal) in 7 days after drug withdrawal.
3.4.3 Relapse rate: after drug withdrawal, in 5 days, clinical symptoms increases the weight of or death.
3.4.4 invalid: unchanged or increase the weight of or dead or disease relapse in duration of test (after comprising drug withdrawal in 5 days) clinical symptoms.
4, result of the test
To commodity mycoplasma pneumoniae of swine therapeutic outcome in table 1.
The therapeutic outcome of table 1 commodity mycoplasma pneumoniae of swine compares
5, test result analysis and conclusion
5.1 as can be seen from above-mentioned result of the test, and total therapeutic effect of tilmicosin pre-mixing agent is much better than matched group medicine.
5.2 tilmicosin pre-mixing agent treatment commodity mycoplasma pneumoniae of swine effects are better than matched group medicine, significant difference.The cure rate of tilmicosin pre-mixing agent also reaches more than 80%, illustrates that this cause of disease is more responsive to tilmicosin pre-mixing agent.But compare control drug, no matter the present invention is that effective percentage or cure rate are all better than control drug, illustrates that the present invention can improve the drug effect of this medicine.
5.3 tilmicosin pre-mixing agents of the present invention can reach desirable therapeutic effect by mixing to feed to pig.
Experimental example 2 tilmicosin pre-mixing agent stability test
This experiment is by the obtained three batches of tilmicosin pre-mixing agents of embodiment 2 formula, carried out stability study according to Ministry of Agriculture's " veterinary drug stability test technical specification (trying) " to it, object is to check tilmicosin pre-mixing agent provided by the invention to light, heat, wet stability.
1. materials and methods
1.1 main agents
Dibutyl amine (chemical analysis is pure) Beijing chemical reagents corporation
Acetonitrile (chromatographically pure) Beijing chemical reagents corporation
Oxolane (chromatographically pure) Beijing chemical reagents corporation
Phosphoric acid (chemical analysis is pure) Beijing chemical reagents corporation
Tilmicosin reference substance (content 50.98%) China Veterinary Drugs Supervisory Inst.
By three batches of tilmicosin pre-mixing agents that embodiment 2 formula is obtained.
1.2 key instrument
High performance liquid chromatograph (HPLC) LC-10A Japan Shimadzu
Xin Hua paper mill, qualitative filter paper middling speed Q/ZHJ3017-91 Hangzhou
CX-100 ultrasonic cleaner Beijing armarium two factory
Precision acidity meter (PHS-3C) Shanghai Lei Ci instrument plant
2XZ-1 type rotary-vane vaccum pump Jinggong Vacuum Equipment Plant, Linhai City
BP310S trace semimicro-analy-tical balance, Sartorius company of BP211D analytical balance Germany
The automatic dual pure water distillator Shanghai glass apparatus company of D1810C
Instrucment and meter plant of JD-3 type illumination meter Shanghai International Automobile City Tourist Festival student's federation
Huangshi medical apparatus and instruments factory of water isolation type electro-heating standing-temperature cultivator GSP-781 type Hubei Province
The detection method of tilmicosin content in 1.3 tilmicosin pre-mixing agents, detects with reference to Ministry of Agriculture's quality standard.
1.4 acceleration by light tests
By the obtained three batches of tilmicosin pre-mixing agents of embodiment 2 formula, represent with No. 1, No. 2, No. 3 respectively, obtained each finished product is loaded in colourless airtight plastic bottle, putting illumination is place 10 days under the condition of 4500 ± 500LX, respectively at 0,5,10 day timing sampling, the indexs such as working sample character, graininess, tilmicosin content.
1.5 heating and moistening tests
According to " Ministry of Agriculture's veterinary drug stability techniques specification (trying) ", determine that this preparation should be 30 ± 2 DEG C in temperature, relative humidity is carry out heating and moistening test under the condition of 60 ± 5%.Sodium nitrite saturated solution is adopted to be humidizer, be placed in bottom exsiccator, the sample plastic bag sealing of each three batches is placed on the upper strata of exsiccator, put into water isolation type electro-heating standing-temperature cultivator in the lump, temperature regulating to 30 ± 2 DEG C, monthly sample once, routine observation 6 months, the indexs such as working sample character, graininess, the uniformity, tilmicosin content.
2, results and analysis
2.1 acceleration by light tests
Acceleration by light result of the test is in table 2.Result shows, said preparation was 4500 ± 500LX strong illumination 10 days, and graininess, tilmicosin content, character have no significant change.
Table 2 acceleration by light result of the test
2.2 heating and moistening tests
Through heating and moistening test, have no significant change at 1 month, 2 months, 3 months, 4 months, 5 months, 6 months its appearance luster, graininess, content, result shows, this compound preparation is to heating and moistening good stability.The results are shown in Table 3.
Table 3 is heated accelerated test result for six months
3, brief summary and discussion
The requirement of this experimental evidence Ministry of Agriculture in 1999 No. 13 files " veterinary drug stability test technical specification (trying) ", under the condition of intense light irradiation, investigates the project such as tilmicosin content, appearance character, graininess of said preparation.Result of the test shows, test 10 days in acceleration by light, indices meets the requirements, and illustrates that this preparation is relatively stable to illumination.
The requirement of this experimental evidence Ministry of Agriculture in 1999 No. 13 files " veterinary drug stability test technical specification (trying) ", under the condition of high temperature, high humility, the project such as tilmicosin content, appearance character, graininess, the uniformity of said preparation is investigated.Result of the test shows, at 6 the end of month of heating and moistening stability test, the appearance luster of preparation significant change does not occur, and all the other indices are normally, meets the requirement of " middle Chinese republic veterinary drug allusion quotation ", and therefore, the environment of high humidity, high heat is still stable.
In sum, tilmicosin pre-mixing agent provided by the present invention to light, heat, wet be all stable.
Although above the present invention is described in detail with a general description of the specific embodiments, on basis of the present invention, can make some modifications or improvements it, this will be apparent to those skilled in the art.Therefore, these modifications or improvements without departing from theon the basis of the spirit of the present invention, all belong to the scope of protection of present invention.
Claims (10)
1. a tilmicosin pre-mixing agent, is characterized in that, by percentage to the quality, containing following component: tilmicosin 5%-50%, and binding agent 0.5%-20%, antioxidant 0.05%-2%.
2. tilmicosin pre-mixing agent according to claim 1, is characterized in that, by percentage to the quality, containing following component: tilmicosin 8%-30%, and binding agent 1%-10%, antioxidant 0.1%-1.5%.
3. tilmicosin pre-mixing agent according to claim 2, is characterized in that, by percentage to the quality, containing following component: tilmicosin 10%-20%, and binding agent 2%-4%, antioxidant 0.5%-1%.
4. the tilmicosin pre-mixing agent according to any one of claim 1-3, is characterized in that, described tilmicosin is the mixture of one or more in tilmicosin, tilmicosin salt.
5. the tilmicosin pre-mixing agent according to any one of claim 1-3, is characterized in that, described binding agent is the mixture of one or more in agar, starch slurry, cellulose derivative, and described binding agent is preferably agar.
6. the tilmicosin pre-mixing agent according to any one of claim 1-3, it is characterized in that, described antioxidant is the mixture of one or more in sodium sulfate, sodium sulfite, sodium sulfite, sodium pyrosulfite, and described antioxidant is preferably sodium sulfite.
7. the tilmicosin pre-mixing agent according to any one of claim 1-6, is characterized in that, also comprise diluent; Described diluent is preferably one or more in starch, dextrin, lactose, sucrose.
8. tilmicosin pre-mixing agent according to claim 7, is characterized in that, described diluent is starch, gathers to total amount to 100% with described diluent starch.
9. the preparation method of tilmicosin pre-mixing agent described in any one of claim 7-8, comprises the steps:
1) get suitable quantity of water and dissolve antioxidant, for subsequent use;
2) to step 1) obtained by solution in add binding agent, stir, for subsequent use;
3) to step 2) obtained by solution in add tilmicosin and stir, add diluent, granulate after making soft material, dry, sieve, to obtain final product.
10. the preparation method of tilmicosin pre-mixing agent described in claim 9, comprises the steps:
1) the water dissolution antioxidant of antioxidant quality 50-60 is got, for subsequent use;
2) to step 1) obtained by solution in add binding agent, stir, for subsequent use; When selecting agar to be binding agent, needing to be heated to 60-80 DEG C, agar is dissolved; 50-60 DEG C is cooled to after stirring;
3) to step 2) obtained by solution in add tilmicosin and stir, add diluent, granulate after making soft material, in 60-80 DEG C of drying, with No. 2 sieves or No. 4 sieved sieves, to obtain final product.
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