固相萃取-高效液相色谱串联质谱法同时测定有机肥料中13种抗生素残留

摘要

建立了同时测定有机肥料中磺胺类、四环素类和喹诺酮类13种抗生素残留的高效液相色谱-串联质谱法,并对样品的前处理方法、仪器分析参数进行了优化.结果表明,13种抗生素在50～1 000 ng/mL间线性关系良好,相关系数均达到0.999以上,检出限在0.02～0.04 mg/kg,样品加标回收率在69％～111％之间,具有良好的重现性.该方法具有灵敏度高、准确度高等优点,可用于有机肥料中13种抗生素残留的同时检测.运用该方法在有机肥料实际检测中发现恩诺沙星、诺氟沙星、土霉素等抗生素残留.%A HPLC-MS/MS method has been developed for simultaneous determination of 13 kinds of antibiotics residues(sulfamerazine,sulfamethazine,sulfadiazine,sulfameter,sulfadimethoxine,sulfamethoxazole,tetracycline,oxytetracycline,chlortetracycline,doxycycline,norfloxacin,enrofloxacin and lomefloxacin)in organic fertilizers.Sample pretreatment method and instrumental analysis parameters had been optimized.The results showed that the method had perfect linearity and repeatability between 50～1 000 ng/mL and the correlation coefficients R was more than 0.999.The detection limits were between 0.02～0.04 mg/kg,and the recoveries were in the range of 69％～111％.The method had the advantages of high sensitivity and high accuracy,so it could be used for simultaneous determination of 13 kinds of antibiotics residues in organic fertilizers.By this method,enrofloxacin,norfloxacin and oxytetracycline were detected in the actual samples of organic fertilizers.