Rapid, sensitive and selective detection of glyphosate in wheat and rice flour using a polar stationary phase by LC-MS/MS.

Rapid, sensitive and selective method was studied for the determination of glyphosate in rice and wheat flour using a Raptor Polar column. Samples were extracted with acidified methanol solution. Isotope labeled internal standard was added with the extraction solvent to ensure accurate tracking and quantitation.

Pesticides and their metabolites in human urine: development of multi-analyte method by LC-MS/MS and GC-MS/MS.

The objective of this study consists of being able to develop a precise, reliable, easy, cheap and quick method to identify and quantify the presence of pesticide metabolites and their parents in human urine. In order to reach our purpose we selected the pesticides and their metabolites with intended uses on permanent crops such as orchards and vineyard. The activity planning started with the identification of the target list carried out by UHPLC-MS/MS and GC-MS/MS, succeeded by several tests oriented to determine the best sample treatment having recourse to instrumental analysis in the range 5-100 ng/mL.

Estimation of the validation parameters for a fast analysis of herbicide residues by LC-MS/MS.

Due to strict regulatory requirements for pesticide residue analysis, only the results of residue analysis with acceptable quality should be reported. As a consequence proper validation of the measurement method is required. In this context, accuracy, precision, specificity, limit of determination (LOQ), matrix effect, linearity, uncertainty calculation and ruggedness become increasingly important.

Uncertainty estimation in the analysis of pesticide residues in olive oil using data from proficiency tests.

In this work we report the results for estimating the measurement uncertainty (MU) following up the application of two different approaches, relatively the top-down procedure, by using proficiency test data. We have focused the estimation on the olive oil matrix. We used the analytical data obtained from five selected editions of the Proficiency Tests (PTs, from 2007 to 2011) on pesticide residues in olive oil to estimate the MU.

Estimation of measurement uncertainty associated to the determination of pesticide residues: a case study.

In the analytical analysis the measurement uncertainty is a quantitative indicator of the confidence describing the range around a reported or experimental result within which the true value can be expected. Several approaches can be used to estimate the measurement uncertainty associated to the analysis of pesticide residues: a) the top-down, the estimation can be referred to default values; b) the bottom-up the estimation is related to the uncertainty sources. Concerning the bottom-up approach, the following contributions have been investigated: weight of sample, calibration solutions, final volume of sample and intermediate repeatability studies.