Simultaneous Detection of Six Herbicides in Blood by QuEChERS-High Performance Liquid Chromatography-Quadrupole-Time of Flight Mass Spectrometry with Positive and Negative Ion Switching Mode
An analytical method based on QuEChERS-high performance liquid chromatography-quadrupole-time of flight mass spectrometry was developed for the determination of six herbicides,including Clopyralid,Mesotrione,Trifloxysulfuron,Triclopyr,Flumioxazin,Benazolinethyl in blood.The samples were extracted with acetonitrile by vortex oscillation,and the extracts were purified by the optimized QuEChERS method and filtered by 0.22 μm filter membrane.The chromatographic separation was achieved on a ZORBAX Eclipse Plus C18 column(100 mm× 3.0 mm,1.8 μm)with a gradient elution of 0.1%formic acid aqueous solution and acetonitrile as the mobile phases,and the detection was switched between positive and negative ions by quadrupole-time of flight mass spectrometry.The linear correlation coefficient of the six herbicides were greater than 0.9981,the limit of detection(LODs)were in the range of 0.02-1.95 μg/L and the limit of quantification(LOQs)were in the range of 0.07-6.49 μg/L.The recoveries of six herbicides were in the ranges of 88.19%-105.19%at the two spiked levels of 100 and 500 μg/kg.The intra-sample precisions were between 0.39%-1.65%.The intra-day precisions were between 0.81%-2.93%,and the inter-day precisions were between 0.08%-2.85%.This method has fast sample pretreatment speed,high sensitivity,good stability and high accuracy,which can meet the qualitative and quantitative analysis needs of herbicide components in blood.It can provide reference for the testing of biological samples in herbicide poisoning cases.
High Performance Liquid chromatographyQuadrupole-time of flight mass spectrometryPositive and negative ion switching modeBloodHerbicide