Rapid screening and confirmation of 11 pesticide residues in fruit by ultra performance liquid chromatography coupled with quadrupole time of flight mass spectrometry
Objective To establish a method for rapid screening and confirming 11 kinds of pesticide residues in fruit by ultra high performance liquid chromatography coupled with quadrupole time of flight mass spectrometry.Methods An accurate mass database at the first level and a fragment ion spectrum at the second level with 10,20,40 V were established.The various fruit samples were pretreated with QuEChERS method,and the optimized mass spectrometry and chromatography conditions were employed.The results were screened by comparing the accurate mass,isotope distribution and abundance,confirmed by comparing the Target MS/MS result in the database.The qualitative analysis was based on software scores,and the quantitative analysis used external standard method.Results There was good linear relationship for the 11 pesticides within the range of 0.2-200.0 μg/L(r≥ 0.999).The detection limit was between 0.2-5.0 μg/kg.Adding low-level,medium-level and high-level standard(5.0,10.0,50.0 μg/kg,respectively),the average recoveries(n=6)were between 91.2％-115.2％,and the relative standard deviations were less than or equal 15.0％.The method was applied to 60 samples of fruits for the screening and confirmation.None of pesticides exceeded the limit according to National Food Safety Standard-Maximum Residue Limits for Pesticides in Food(GB 2763-2021).Conclusions This method has the advantages of high efficiency,high throughput,and high sensitivity;the quantitative results are accurate and reliable;the 11 pesticides can be screened and confirmed in a short time and in the absence of standards.
Ultra high performance liquid chromatography coupled with quadrupole time of flight mass spectrometryFruitPesticide residues
NETL
NSTL
万方数据
