The Quality Standard of Quinocetone.doc

The Quality Standard of QuinocetoneKuixitongQuinocetone 18H14N2O3 306.32 Quinocetone is called 3-methyl-2-cinnamicacyl-quinoxalinee-1, 4-dioxide in chemistry. The content of C18H14N2O3 is no less than 98.0% in drying .Character The drug is yellow crystalline or amorphous powder, and has no abnormal flavour. It could be easily dissolved in CHCl3, dioxane and dimethyl sulfoxide, and slightly in methyl alcohol and ethyl alcohol but not in water. Melt point Melt point of the drug is 190-193.0 (based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 34 ), melting coincided with disintegration.Identification (1) After 0.2g of the drug is weighed approximately and dissolved with 10ml dimethyl formamide completely, 2mL of the solution is taken out to tube and then 2 drops of 1% KMnO4 solution is added. On shaking, the colour with KMnO4 fades and fuscescent sediment emerges.(2) 50mg of the drug is accurately put into a 100mLamber-coloured volumetric flask. After dissolved with 10mL dioxane, the solution is diluted by 40% dioxane to the scale. On shaking completely, 1ml of the solution is measured accurately and put into 50mL amber-coloured volumetric flask. Assaying based on spectrophotometric method (based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 17 ), the results indicate that the solution has maximum absorption value at 2311nm,2601nm, 3141nm wavelength.(3) Absorption spectrum of infrared spectrum should be in accord with comparison spectrum. Examination Chloride 0.2g of the drug is weighed and 10mL water is added. The solution is heated until boiling, and then is cooled to room temperature. After crystal is separated completely, the solution is filtered and added with water to 50mL. The solution is divided into two parts. Based on determination method(based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 51 ) and compared with standard sodium chloride solution, chloride of the drug is no more than 0.05%.Related substance CHCl3 is added to the drug in order to prepare 10mg/mL solution for test. The solution is measured accurately and diluted with CHCl3 to 0.05mg /mL as comparison solution. The two above solutions should be prepared before used. Based on thin-layer chromatography (based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 23), 10ml of the above two solutions is absorbed and pointed separately on the identical thin layer plate of silica gel GF254. The sample is expanded at dark place with CHCl3-acetone (41) as a developing solvent. On open-air drying, the thin layer plate of silica gel GF254 is inspected under the viltalight lamp. If the impure spots is discovered in the prepared solution, the color of impure spots is less dark in comparison with main spots of comparison solution.Loss on drying The product is dried at 105 until it is constant weight. Loss in weight is no more than 0.3% (based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 57). Ignition residue The residue after ignition is no more than 0.2%( based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 59 ).Heavy metal The content of the heavy metal in the ignition residue is no more than 20 of million ( based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 54 ).Arsenic salt 1g of the drug is mixed with 1g Ca(OH)2 and then a little of water was added. After stirred uniformly and dried, the mixture is burn with weak fire to carbonization fully at 500-600. After cooling, 5mL hydrochoric acid and 3ml water are added in order to dissolve the residue. The content of the arsenic is no more than 2 of million ( based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 56 ).Assaying Based on high performance liquid chromatography ( in Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 24).Chromatographic condition and system suitability experiment Octadecyl silane linkage silica gel is used as bulking agent. Methyl alcohol-water (6040) is used as mobil phase, detection wavelength is 314m and the number of theoretical plates calculated with quinocetone is no less than 3000. Assaying After the sufficient product is weighed accurately, DMF is added to 2mg of quinocetone per mL. The solution is diluted with methyl alcohol to 0.1mg/mL. Then 10L of the solution is measured accurately and input to chromatograph of liquid, then chromatogram is recorded. The comparison sample of quinocetone with constant weight at 105 is determined as the above. The content is calculated with peak area by external reference method.Effect and usage antibacterial drug, growth promoter in livestock and poultry.Direction and dosage the product is used as a feed additive.Per 1000kg stoyer pig: 50g (50ppm); adult fowl: 75g (75ppm), chicken: 50g (50ppm). The addition of the other fowls and livestock was the same to the above. It must be uniform when quinocetone is added to stoyer.Store away from light, closeed tightly, reserved at the dry places.Preparation premix of quinocetoneThe Quality Standard of Quinocetone Premix Quinocetone premix is made of both quinocetone and light qualitative CaCO3 , the content of quinocetone in premix is 90.0-110.0% of regulation quanity. Identification (1) After the premix including 0.2g quinocetone is weighed approximately and dissolved with 10ml dimethyl formamide completely, 2mL of the solution is taken out to tube and then 2 drops of 1% KMnO4 solution is added. On shaking, the colour with KMnO4 fades and fuscescent sediment emerges.(2) The solution in assay condition is measured. Assaying based on spectrophotometric method (based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 17 ), the results indicate that the solution has maximum absorption value at 2311nm,2601nm, 3141nm wavelength.Examination Loss on drying The product is dried at 105 until it is constant weight. Loss in weight is no more than 3% (based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 57).Others should be according with every regulation of premix (based on Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 11)。Assaying Based on high performance liquid chromatography ( in Veterinary Pharmacopoeia of China, the first supplement, editon 2000, page 24).Chromatographic condition and system suitability experiment Octadecyl silane linkage silica gel is used as bulking agent. Methyl alcohol-water (6040) is used as mobil phase, detection wavelength is 314m and the number of theoretical plates calculated with quinocetone is no less than 3000. Assaying After the sufficient product is weighed accurately to Erlenmeyer flask with lid, methyl alcohol is added to 20g of quinocetone per mL. The filtering solution at first is given up and the continuous sol