高效液相色谱荧光检测法同时检测鸡肉中氟苯尼考及氟苯尼考胺残留

经丙酮、二氯甲烷提取,饱和正己烷脱脂,氮吹仪吹干浓缩后,以乙腈-磷酸二氢钠溶液(0.01 mol/L,含0.005mol/L十二烷基硫酸钠和0.1%三乙胺)(35 :65)为流动相,流速为1.0 mL/min,荧光检测激发波长为225 nm,发射波长285 nm.氟苯尼考在0.01～10.0 mg/L、氟苯尼考胺在0.002 5～2.5 mg/L浓度范围内,本方法线性关系良好,相关系数分别为0.999 7和0.999 8.当添加水平氟苯尼考为15～500 μg/kg、氟苯尼考胺为5～500μg/kg时.该方法平均回收率分别为79.5%～84.6%和80.7 0A～88.2%,相对标准偏差分别为2.8%～6.4%和2.4%～5.3%;检测限分别为5μg/kg和μg/kg.该方法样品处理简单,可同时检测氟苯尼考和氟苯尼考胺的残留,且准确度和精密度均符合残留分析的要求.

Simultaneous determination of residues of forfenicol and forfenicol amine in chicken muscle by HPLC with fluorescence detection

A high performance liquid chromatography with fluorescence detection method was developed for simulta-neous determination of residues of forfenicol(FF) and forfenicol amine(FFA) in chicken muscle.Forfenicol and for-fenicol amine were extracted with acetone and dichloromethane from chicken muscle.The extract was rinsed with n-hexane saturated with acetonitrile and dried with nitrogen evaporator,The mobile phase was acetonitrile-sodium di-hydrogen phosphate solution(0.01 mol/L,containing 0.005 mol/L SDS and 0.1% triethylamine) (35 : 65,by vol-ume) ,the flow rate was 1 mL/min.The fluorescence detection with an excitation wavelength of 225 nm and an emis-sion wavelength of 285 nm.The linear ranges were 10-10 000μg/L of florfenicol and 2.5-2 500μg/L of florfenicol a-mine,respectively.The correlation coefficient was 0.999 7 for florfenicol and 0.999 8 for fiorfenicol amine,respec-tively.At spiked level 15-500μg/kg for florfenicol and 5-500μg/kg for florfenicol amine,recoveries were 79.5 %-84.6% and 80.7%-88.2% ,respectively,with relative standard deviations from 2.8%-6.4% and from 2.4%-5.3% ,re-spectively.The detection limits were 5 μg/kg for florfenicol and 1 μg/kg for florfenicol amine.This method meets the demand of residues determination of florfenicol and florfenicol amine.