乐山地区特种黑鸡鸡肉中十四种磺胺类药物残留量的测定研究

Study on the Determination of 14 Kinds Sulfonamides Residues in Chicken Meat in Leshan

建立了乐山地区特种黑鸡鸡肉中磺胺类药物残留的HPLC的检测方法。以GB 29694-2013《食品安全国家标准动物性食品中13种磺胺类药物多残留的测定高效液相色谱法》~[1]为基础进行实验,鸡肉中的药物残留用乙酸乙酯溶液提取,后采用混合型阳离子交换固相萃取柱Cleanert PCX进行净化。分析样品以甲酸(体积分数为0.1%)和乙腈溶液为流动相,流速1mL/min,检测波长270nm,柱温40℃,进样量10μL,经ODS-3 C18色谱柱分离,在HPLC方法下进行测定分析。结果显示:方法简单易行,前处理效果理想,磺胺类的测定在10-500?g/L范围内具有良好的线性关系,相关系数基本满足r>0.999。在20μg/kg的加标水平下,14种磺胺类药物的平均回收率为80-110%,相对标准偏差为0.9-10%,检测限为5-10μg/kg。

To establish the sulfonamides residues in Leshan＇s special black chicken and testing method of HPLC.Refer to GB 29694-2013 《National food safety standards more than 13 kinds of sulfa drugs residues in animal foods high performance liquid chromatography（HPLC） for determination of the law》-[1], the 14 samples of chicken extracted with ethyl acetate solution; After using cationic exchange of solid phase extraction column Cleanert PCX for purification. Analysis of samples with formic acid（volume fraction is 0.1%） and acetonitrile solution as mobile phase, flow rate of 1 m L/min, detection wavelength of 270 nm, column temperature 40℃, sample quantity 10μL：by the ODS-3 C18 chromatographic column separation, down in the HPLC method to determine analysis. The results showed that the determination of sulfonamides in the range of 10-500μg/L has a good linear relationship, the correlation coefficient basically meet the r0.999. The average recoveries at spiked concentration level of 20μg/kg ranged from 80% to 110%, with relative standard deviations（RSDs） of 0.9-10%. The detection limits ranged from5μg/kg to 10μg/kg.