渔稻共作模式下稻谷中农药(包含代谢物)和抗生素残留量检测方法

Simultaneous Determination of Pesticides(Including Metabolites)and Antibiotics Residues in Paddy by Co-cultivation of Fish and Rice

为建立一种稻谷中农药(包含代谢物)和抗生素高通量检测方法,通过简单快捷的前处理,使用超高效液相色谱-三重四极杆质谱(6495 Triple Quadrupole LC/MS System)检测57种化合物。样品经Mcllvaine-Na2 EDTA缓冲液充分润湿、乙腈提取,无水硫酸钠吸附水分,离心分层,过有机相微孔滤膜净化。液质联用仪采用甲酸水溶液(A)和乙腈溶液(B)作为流动相进行梯度洗脱,质谱(ESI)采用多离子动态检测模式(dMRM)对57种农药和抗生素的定量离子和定性离子进行了监测。结果表明:在12 min内完成57种目标化合物的分离分析。57种农药和抗生素在2、4和20μg/kg(四环素类10、20、100μg/kg)添加水平的回收率为:60.01%~118.10%,相对标准偏差:0.04%~19.62%,相对标准偏差小于20.0%(n=6),方法定量限为1μg/kg(四环素类5μg/kg)。该方法快速、准确、灵敏,适合测定稻谷中农药(包含代谢物)和抗生素微量残留。

This paper is to determine 57 pesticides(including metabolites)and antibiotics in paddy by liquid chromatography-tandem mass spectrometric(6495 Triple Quadrupole LC/MS System)and with identical pretreatment.Paddy samples were wetted with Mcllvaine-Na2 EDTA buffer solution,extracted with acetonitrile,adsorbed moisture with anhydrous sodium sulfate,separated by centrifuging and cleaned up by organic phase microporous filter membrane.And then the 57 pesticides(including metabolites)and antibiotics were separated on a reversed phase using a gradient elution program of formic acid aqueous solution(A)and acetonitrile solution(B).LC-MS/MS(ESI)adopt dynamic multiple reactions monitoring(dMRM).Identification of the major components of the pesticides(including metabolites)and antibiotics residues was performed based upon the intensities of fragments.Results:The recoveries were ranged from 60.01%to 118.10%for the 57 pesticides(including metabolites)and antibiotics residues with 3 spiked levels of 2,4 and 20μg/kg(tetracyclines 10,20 and 100μg/kg).The relative standard deviations(RSDs)were less than 20.0%(n=6),and the limits of quantitation(LOQ)for the 53 kinds of pesticedes(including metabolites)and antibiotics were 2μg/kg(tetracyclines 10μg/kg).The proposed method is fast,accurate and sensitive,which is suitable for detecting 57 pesticides(including metabolites)and antibiotics in paddy.