固相萃取–高效液相色谱法同时测定饲料中4种磺胺类药物残留

建立固相萃取–高效液相色谱法同时测定饲料中的磺胺嘧啶、磺胺二甲嘧啶、磺胺甲恶唑、磺胺喹恶啉4种磺胺类药物残留的方法。样品用乙腈提取,然后用碱性氧化铝固相萃取柱净化,色谱柱为C_(18)柱(250 mm×4.6mm,5μm),以水–乙腈(体积比为75∶25,含0.3%乙酸)为流动相,流量为1.0 mL/min,检测波长为270 nm。4种磺胺类药物的质量浓度在1~10μg/mL范围内与其色谱峰面积呈良好的线性,相关系数均大于0.999,检出限为0.025~0.133μg/g。磺胺类药物测定结果的相对标准偏差为0.22%~0.30%(n=6),样品加标回收率为93.6%~106.7%。实际饲料样品中均未检出这4种磺胺组分。该方法具有干扰少,灵敏度高,重复性好的优点,可以作为饲料中的磺胺类药物残留的一种检测方法。

Simultaneous Determination of Four Suifonamide Residues in Feeds by High Performance Liquid Chromatography with Solid Phase Extraction

A method was developed for simultaneous determining sulfadiazine, sulfadimidine, sulphamethoxazole, sulfaquinoxaline in feeds by high performance liquid chromatography with solid phase extraction. The feed sample was extracted by acetonitrile and then purified with Cleanert Alumina-B Solid Phase Extraction column,and separated on C18 colunm(250 mm×4.6 mm,5 μm) by using mobile phase of acetonitrile-water (volume ratio was 75:25,with 0.3％ acetic acid) at flow rate of 1.0 mL/min,then detected at 270 nm. The concentration of four suifonamide residues had good linear relationships with the chromatographic peak area in the range of 1-10 μg/mL,the correlation coefficients were more than 0.999, the detection limits were 0.025-0.133 μg/g. The relative standard deviation of determination results was 0.22％-0.30％(n=6). The average recoveries were in the range of 93.6％-106.7％. The four suifonamide residues were not determined in actual feed samples. This method has the advantages of less interference, high sensitivity,good repeatability, and it is suitable for the determination of four sulfonamides in feeds.