Article ID | Journal | Published Year | Pages | File Type |
---|---|---|---|---|
8850826 | Chemosphere | 2018 | 36 Pages |
Abstract
In this study, we developed a multiresidue method for the analysis of 310 pesticides in representative agricultural produce (brown rice, orange, and spinach) using ultra high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) combined with a modified QuEChERS procedure. The optimal mobile phase composition (Methanol containing 5â¯mM ammonium formate and 0.1% formic acid) produced high sensitivity and reliable results. Also, the relationship between injection volume and repeatability of peak area was investigated. Most of the target pesticides had a limit of quantitation under 10â¯ngâ¯gâ1, and correlation coefficients (r2)â¯>â¯0.99 in matrix-matched standards within the range of 1-100â¯ngâ¯gâ1. To validate the optimized method, recovery tests were performed with each of the crops at 10 and 50â¯ngâ¯gâ1 spiking levels (nâ¯=â¯5). Satisfactory recoveries were achieved showing that 86.8-88.7% (at 10â¯ngâ¯gâ1) and 91.9-96.1% (at 50â¯ngâ¯gâ1) of the pesticides met the validation criteria (recoveries in the range of 70-120% and relative standard deviationâ¯â¤â¯20%). Fifteen compounds were found to show a loss of recovery due to adsorption by primary and secondary amine or graphite carbon black. In the case of brown rice, 86.1% of pesticides showed an insignificant matrix effect (<±20%), while 35.2% and 41.6% of pesticides in orange and spinach were in that range, respectively. Sixteen apple samples from local markets were analyzed to evaluate the applicability of the optimized method. Nineteen pesticides were detected, of which the concentrations were lower than the maximum residue limit.
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Environmental Chemistry
Authors
Jonghwa Lee, Yongho Shin, Junghak Lee, Jiho Lee, Byung Joon Kim, Jeong-Han Kim,