UPLC-MS/MS法同时快速检测有机肥中55种抗菌药物

Simultaneous and rapid detection of 55 antibacterial drugs in organic fertilizer using UPLC-MS/MS

建立了同时检测有机肥中磺胺类、大环内酯类、喹诺酮类3类55种抗菌药物残留的超高效液相色谱-串联质谱法(UPLC-MS/MS)。将有机肥研磨、过筛制成试验样品后,使用HLB固相萃取柱净化,上样后依次用去离子水、5%乙腈水溶液淋洗,甲醇/乙酸乙酯溶液(体积比7∶3,含5%氨水)洗脱,氮吹吹干,0.1%甲酸水/乙腈(体积比=9∶1)复溶;在多反应检测模式下进行测定,外标法定量。结果表明,4批有机肥中55种药物在1.0~100μg/kg范围内线性关系良好(R2>0.9900),该方法的检出限为2.0~7.5μg/kg,定量限为5.0~25.0μg/kg,各种药物的回收率为60.2%~118.7%,批内相对标准偏差(n=5)为0.5%~15.0%,批间相对标准偏差(n=20)为4.3%~24.1%。该方法简单可靠,净化效果好,适用于有机肥中磺胺类、喹诺酮类、大环内脂类药物的同时检测。

An ultra high performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was established for the simultaneous detection of 55 types of antibacterial drugs,including sulfonamides,macrolides,and quinolones,in organic fertiliz-er.After grinding and sieving the organic fertilizer into experimental samples,they were purified using HLB solid-phase extraction col-umn.After loading,the samples were sequentially washed with deionized water and 5%acetonitrile aqueous solution,eluted with methanol/ethyl acetate solution(volume ratio 7∶3,containing 5%ammonia),blown dry with nitrogen,and re-dissolved in 0.1%for-mic acid water/acetonitrile(volume ratio 9∶1);measurement was carried out in a multi reaction detection mode,with the external stan-dard method for quantification.The results showed that among the four batches of organic fertilizers,55 drugs had a good linear rela-tionship(R2>0.990)within the range of 1.0~100μg/kg,the detection limit of this method was 2.0~7.5μg/kg,the quantitative limit was 5.0~25.0μg/kg,the recovery rates of various drugs were 60.2%~118.7%,the relative standard deviation within the batch(n=5)was 0.5%~15.0%,and the relative standard deviation between batches(n=20)was 4.3%~24.1%.This method was simple and reliable,with a good purification effect,and was suitable for the simultaneous detection of sulfonamide,quinolone,and macrocyclic lipid drugs in organic fertilizer.