Analysis of Pesticide Residues by QuEChERS Method and LC-MS/MS for a New Extrapolation of Maximum Residue Levels in Persimmon Minor Crop

Abstract

According to EU guidance SANCO/7525/VI/95 Rev.10.3, residue data extrapolation from a surrogate major crop to a minor crop can be used for setting maximum residue levels (MRLs) with a reduced number of residue trials and representative selected pesticides. In this work, a QuEChERS method (citrate-buffered version and PSA with MgSO4 clean-up) and LC-ESI-MS/MS for the determination of boscalid, pyraclostrobin, fludioxonil, fluopyram and tebuconazole in persimmon was developed and validated according to EU Commission guidelines and afterwards used for the determination of residues in four field trials. Residue levels at harvest for each pesticide ranged between 0.347 and 0.028 mg/kg. After comparing EFSA residue data on apples, as the surrogate major crop, and conducting a consumer risk assessment, a proposal of residue data extrapolation to set MRLs in persimmons was performed. The results showed that pesticide residues in persimmons at harvest were consistently lower than residues in apples when substances were applied according to the same critical GAP. MRLs were set at 0.5 mg/kg for fludioxonil, 0.6 mg/kg for boscalid, 0.3 mg/kg for tebuconazole, 0.4 mg/kg for fluopyran and 0.3 mg/kg for pyraclostrobin. The ratio of the MRLs for apple/persimmon varied between 2.5 for boscalid and 1.25 for fluopyram, suggesting that residue extrapolation can be feasible, promoting the process of pesticide registration for minor crops and the settlement of MRL.

Multi-Residue Screening of Pesticides in Aquatic Products Using High-Performance Liquid Chromatography-Tandem High-Resolution Mass Spectrometry

“…For some pesticides, a certain amount of acid in the extractant may be beneficial to the stability of the pesticide [ 26 ]. In our work, Dodemorph, xylazine, robenidine, phorate and avermectin B1a may be extracted with greater than 20% recoveries using 0.5% or 1% formic acid acetonitrile, according to the experiment’s results ( Figure 2 ).…”

Development of Analytical Methods to Analyze Pesticide Residues

“…Sandín-España et al [ 9 ] developed and validated a QuEChERS method (citrate-buffered version and PSA with MgSO4 clean-up) followed by LC-ESI-MS/MS for the determination of different class pesticides in persimmon. The method was developed and validated according to EU Commission guidelines and afterwards used for the determination of residues in four field trials.…”

Dissipation Residue Behaviors and Dietary Risk Assessment of Boscalid and Pyraclostrobin in Watermelon by HPLC-MS/MS

“…However, in recent studies, very few methods have been developed to detect the two drugs together [ 13 , 26 ]. Single-drug assays are easier to develop because of their simpler instrument development methods [ 27 , 28 , 29 , 30 , 31 , 32 ]. Therefore, this study developed an LC-MS/MS technique that can detect boscalid and pyraclostrobin simultaneously, which optimized the drug retention time and greatly shortened the detection time.…”