摘要
建立了高效液相色谱荧光法同时检测鸡肉中甲砜霉素、氟苯尼考和氟苯尼考胺残留的新方法。样品经丙酮、二氯甲烷提取,饱和正己烷脱脂,氮吹仪吹干浓缩后,以乙腈-NaH2PO4溶液(0.01 mol/L,含0.005 mol/L十二烷基硫酸钠和0.1%三乙胺)(体积比32:68)为流动相,流速为1.0 mL/m in,荧光检测激发波长为225nm,发射波长为290 nm。甲砜霉素、氟苯尼考和氟苯尼考胺均在0.01～1.75 mg/L浓度范围内线性关系良好,相关系数分别为0.9991、0.9989和0.9994。当甲砜霉素、氟苯尼考、氟苯尼考胺添加水平均为5～500μg/kg时,方法平均回收率分别为78.5%～88.7%、79.3%～82.5%和80.5%～85.6%;检测限分别为1.5、1.5、0.5μg/kg(S/N=3);定量限分别为5、5、2μg/kg(S/N=10)。该方法可同时检测鸡肉中甲砜霉素、氟苯尼考和氟苯尼考胺的残留。
A high performance liquid chromatography with fluorescence detection method（HPLC-FLD） was developed for simultaneous determination of residues of thiamphenicol（TAP）,forfenicol（FF） and forfenicol amine（FFA） in chicken muscle.TAP,FF and FFA in chicken muscle were extracted with acetone and dichloromethane.Extraction 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 by volume）,and the flow rate was 1.0 mL/min.The fluorescence detection was performed at an excitation wavelength of 225 nm and an emission wavelength of 290 nm.The linear ranges were all 0.01~1.75 mg/L.The correlation coefficients were 0.9991 for TAP,0.9989 for FF and 0.9994 for FFA,respectively.At spiked levels of 5~500 μg/kg for TAP,FF and FFA,recoveries ranged from 78.5% to 88.7%,79.3% to 82.5% and 80.5% to 85.6%,respectively.The detection limits were 1.5 μg/kg for TAP,1.5 μg/kg for FF and 0.5 μg/kg for FFA（S/N=3）,respectively.The lowest quantitative limits were 5 μg/kg for TAP,5 μg/kg for FF and 2 μg/kg for FFA（S/N=10）,respectively.This HPLC-FLD method is simple,rapid,high sensitivity and meets the demand of simultaneous determination of residues of TAP,FF and FFA in chicken muscle.
出处
《分析试验室》
CAS
CSCD
北大核心
2011年第7期31-35,共5页
Chinese Journal of Analysis Laboratory
基金
国家肉鸡产业技术体系(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)资助
