| A experiment selected to 1-days-old chickens to raise from Ji li De da farm,and randomly divided into 3groups,every group contained 20 chickens. The 3 groups were the control group, the adding experiment group,and sampling experiment group. After 7 weeks,the tissues samples were taken from the chickens ,doing deferent deal and detecting the tissues.HPLC with pre-column derivatisation and ultraviolet detection was used to detect streptomycin residues in chicken tissues. Detection conditions of HPLC and disposal method of sample including the proportion and speed of mobile phase, dosage of solution and elution were optimized. The setting of method included the selection of derivative reagent,conditions of derivative and detection wavelength, the studying of stability of derivative product,setting of conditions of HPLC,the making of Standard Charts and recovery experiment.The setting of conditions of HPLC included the proportion and speed of mobile phase,PH of Buffer fluid, emperarure of colum and quantity of injection.(l)The results showed that 1,2- beta consignment -4- Huangsuanna and Sodium hydroxide were the best derivative reagent by testing.The response is completely in 10 min of 45 ℃ .And there are identity the largest absorb when the wavelength is 250nm .The derivative product is relatively stable in 5 hour.(2)By screening the conditions of HPLC to all Parameters,The results: There is a best detection condition when the proportion and speed of mobile phase is acetonitrile, acetic acid buffer solution and water (10:10:80), speed is 0.3 mL/min, Buffer fluid PH is 3.3,temperarure of colum is 35℃, wavelength is 252 nm, quantity of injection is 20 μL.(3)The disposal conditions of sample including the selection of precipitant and dosage of eluent The results:Determined the recoveries of three different tissues and different addition concentration using precipitant (5%,5 mL) and eluant(10 mL). The recoveries were 75%~90%, 70%~86% and 64%~75% when addition concentrations were 200 μg/mL, 100 ug/mL, 50 μg/mL. |
