Multiresidue determination of pesticides in crop plants by the quick, easy, cheap, effective, rugged, and safe method and ultra-high-performance liquid chromatography tandem mass spectrometry using a calibration based on a single level standard addition in the sample.

In this study, a QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method, optimized by a 23 full factorial design, was developed for the determination of 72 pesticides in plant parts of carrot, corn, melon, rice, soy, silage, tobacco, cassava, lettuce and wheat by ultra-high-performance liquid chromatographic tandem mass spectrometry (UHPLC-MS/MS). Considering the complexity of these matrices and the need of use calibration in matrix, a new calibration approach based on single level standard addition in the sample (SLSAS) was proposed in this work and compared with the matrix-matched calibration (MMC), the procedural standard calibration (PSC) and the diluted standard addition calibration (DSAC). All approaches presented satisfactory validation parameters with recoveries from 70 to 120% and relative standard deviations≤20%. SLSAS was the most practical from the evaluated approaches and proved to be an effective way of calibration. Method limit of detection were between 4.8 and 48µgkg-1 and limit of quantification were from 16 to 160µgkg-1. Method application to different kinds of plants found residues of 20 pesticides that were quantified with z-scores values≤2 in comparison with other calibration approaches. The proposed QuEChERS method combined with UHPLC-MS/MS analysis and using an easy and effective calibration procedure presented satisfactory results for pesticide residues determination in different crop plants and is a good alternative for routine analysis.

Evaluation of the QuEChERS method for the extraction of pharmaceuticals and personal care products from drinking-water treatment sludge with determination by UPLC-ESI-MS/MS.

A modified version of the QuEChERS method has been evaluated for the determination of 21 pharmaceuticals and 6 personal care products (PPCPs) in drinking-water sludge samples by employing ultra high liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). The performance of the method was evaluated through linearity, recovery, precision (intra-day), method detection and quantification limits (MDL and MQL) and matrix effect. The calibration curves prepared in acetonitrile and in the matrix extract showed a correlation coefficient ranging from 0.98 to 0.99. MQLs values were on the ng g(-1) order of magnitude for most compounds. Recoveries between 50% and 93% were reached with RSDs lower than 10% for most compounds. Matrix effect was almost absent with values lower than 16% for 93% of the compounds. By coupling a quick and simple extraction called QuEChERS with the UPLC-MS/MS analysis, a method that is both selective and sensitive was obtained. This methodology was successfully applied to real samples and caffeine and benzophenone-3 were detected in ng g(-1) levels.