通过式固相萃取净化/超高效液相色谱-串联质谱法测定畜禽肉中19种除草剂残留

Determination of 19 herbicides residues in meat by ultra performance liquid chromatography-tandem mass spectrometry with pass-through solid phase extraction

建立了一种快速测定畜禽肉中19种除草剂残留的超高效液相色谱-串联质谱(UPLC-MS/MS)分析方法.样品以乙腈提取,经Oasis PRiME HLB固相萃取柱通过式净化,采用ACQUITY UPLC BEH C18柱(2.1 mm×50 mm,1.7μm)进行液相色谱分离,以乙腈和0.1%甲酸溶液作为流动相进行梯度洗脱.采用电喷雾电离源、正离子模式下以多反应监测(MRM)进行定量分析,以基质配制标准溶液外标法定量.结果表明,19种除草剂在0.2—50μg·L-1范围内线性关系良好(R2>0.999),方法检出限为0.5—2.0μg·kg-1,定量限为1.7—6.7μg·kg-1,在3个添加水平的加标回收率为70.2%—127.5%,相对偏差为4.1%—10.9%.该方法前处理简便快速,且准确性好、灵敏度高,适用于畜禽肉中19种除草剂残留的测定.

An ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)method was developed for the determination of 19 herbicides residues in meat.The samples were extracted with acetonitrile,and purified by pass-through solid phase extraction using Oasis PRiME HLB column.The seperation was performed on an ACQUITY UPLC BEH C18(2.1 mm×50 mm,1.7μm)column with acetonitrile and 0.1%formic acid as mobile phases by gradient elution.The electrospray source was in the positive ion mode and monitored in the multiple reactions monitoring mode.The 19 herbicides showed great linear relationships in the range of 0.2—50μg·L-1 with correlation coefficients(R2)greater than 0.999.The limits of detection(LODs)and limits of quantitation(LOQs)were in the ranges of 0.5—2.0μg·kg-1 and 1.7—6.7μg·kg-1,respectively.The average recoveries of targets varied from 70.2%to 127.5%,and the relative standard deviations were between 4.1%and 10.9%at three spiked levels.The experimental results indicated that the proposed method is simple,quick,accurate and sensitive,and was suitable for the determination of 19 herbicides residues in meat.