摘要
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5~500μg/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5μg/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。
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 500 μg/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.
出处
《中国畜牧兽医》
CAS
北大核心
2011年第3期163-166,共4页
China Animal Husbandry & Veterinary Medicine
基金
国家肉鸡产业技术体系资助(nycytx-42G1-05)
江苏省高新技术计划项目(BG2005307)
江苏省科技成果转化专项(BA2008071)
关键词
高效液相色谱
荧光检测法
甲砜霉素
鸡肉
残留
high performance liquid chromatography（HPLC）
fluorescence detection
thiamphenicol（TAP）
chicken muscle
residues
