Determination of pyridaphenthion in soybean sprout samples by gas chromatography mass spectrometry with matrix matching calibration strategy after metal sieve linked double syringe based liquid-phase microextraction.

A novel analytical strategy for the trace determination of pyridaphenthion pesticide was developed in this study. Gas chromatography-mass spectrometry (GC-MS) was used for the accurate, feasible and precise determination of this analyte. Liquid phase microextraction (LPME) was performed with a metal sieve linked double syringe (MSLDS) system, which eliminated the need for a disperser solvent. In order to increase extraction efficiency for the analyte, all variable parameters were optimized and the system analytical performance of the proposed method was determined. Limit of detection and quantification (LOD and LOQ) values of pyridaphenthion were found to be 0.8 and 2.7 µg L-1, respectively. Compared to GC-MS system's analytical performance, the developed method provided approximately 273-folds improvement in the detection limit of the analyte. Applicability/accuracy of the developed analytical strategy was checked by recovery experiments carried out with soybean sprouts, and the results obtained were satisfactory.

Determination of fipronil and bixafen pesticides residues using gas chromatography mass spectroscopy with matrix matching calibration strategy after binary dispersive liquid-liquid microextraction.

The objective of this study was to determine bixafen and fipronil residues in domestic and industrial wastewater, soil and mint samples by binary dispersive liquid-liquid microextraction method (BDLLME) prior to gas chromatography-mass spectrometry (GC-MS). Extraction efficiency for the selected analytes was improved by optimizing the parameters such as solvent type, ratio and volume, dispersive solvent type/volume, mixing type and duration to increase overall analytical performance. Under the optimum chromatographic and extraction conditions, limits of detection values for bixafen and fipronil were determined as 7.3 and 6.1 µg L-1, respectively. Spiking experiments were performed for domestic and industrial wastewater, soil and mint samples to evaluate applicability and accuracy of the proposed method. Recovery results for the samples were calculated in the range of 89.4%-112.6% via matrix matching calibration strategy. It was determined that the detection power of GC-MS system was improved 7.8 times for bixafen and 119 times for fipronil over LOD comparisons of conventional GC-MS and B-DLLME-GC-MS systems.