高效液相色谱荧光检测法检测鸡肉中甲砜霉素残留

摘要

A high performance liquid chromatography with fluorescence detection(HPLC-FLD) method was built for determination of residues of thiamphenicol(TAP) in chicken muscle.TAP was extracted with acetone and dichloromethane from chicken muscle.Extract solution was degreased with n-hexane and evaporated with nitrogen evaporator, the mobile phase was acetonitrile-sodium dihydrogen phosphate solution(0.01 mol/L, containing 0.005 mol/L SDS and 0.1％ triethylamine)(32 :68) ,the flow rate was 1.0 mL/min.The fluorescence detection was with an excitation wavelength of 225 nm and an emission wavelength of 290 nm.The data showed that the linear relationship of TAP was nice (r=0.9991) in 0.01 mg/L to 1.75 mg/L concentration range.At spiked level 5 to 500μg/kg for TAP, the average recovery ranged from 79.49 ％ to 89.71 ％, relative standard deviation(RSD) ranged from 4.96％ to 9.61％, the within-day RSD ranged from 5.68％ to 7.47％, the between day RSD ranged from 8.89 ％ to 11.32％.The lowest detection limit of TAP was 1.5 μg/kg(S/N=3) and the lowest quantitative limit of TAP was 5 μg/kg (S/N= 10).This HPLC-FLD method is simple, rapid,high sensitivity and suitable for high sensitivity determination of TAP in chicken muscle.%研究建立了用高效液相色谱荧光法检测鸡肉中甲砜霉素残留的方法.鸡肉经丙酮、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0.005 mol/L十二烷基硫酸钠和0.1%三乙胺)(32:68,V/V)为流动相,流速为1.0 mL/min,荧光检测激发波长为225 nm,发射波长为290 nm.甲砜霉素在0.01～1.75 mg/L浓度范围内,本方法线性关系良好,相关系数为0.9991.当甲砜霉素添加水平为5～500 μg/kg时,该方法平均回收率为79.49%～89.71%,相对标准偏差为4.96%～9.61%;日内相对标准偏差为5.68%～7.47%;日间相对标准偏差为8.89%～11.32%.甲砜霉素检测限为1.5μg/kg(S/N=3),定量限5 μg/kg(S/N=10).所建立的方法简便、快速、灵敏度高,适用于鸡肉中甲砜霉素残留的高灵敏度检测.