Determination of Organophosphorus Pesticides in Fruit Juices by Matrix Solid-Phase Dispersion and Gas Chromatography

Abstract

A rapid multiresidue method was developed for the determination of nine organophosphorus pesticides in fruit juices. The analytical procedure is based on the matrix solid-phase dispersion (MSPD) of juice samples on Florisil in small glass columns and subsequent extraction with ethyl acetate assisted by sonication. Residue levels were determined by gas chromatography with nitrogen-phosphorus detection. Spiked blank samples were used as standards to counteract the matrix effect observed in the chromatographic determination. The NPD response for all pesticides was linear in the concentration range studied with determination coefficients >0.999. Average recoveries obtained for all of the pesticides in the different juices and fortification levels were >70% with relative standard deviations of <11%. The detection limits ranged from 0.1 to 0.6 microg/kg. The identity of the pesticides was confirmed by gas chromatography with mass spectrometric detection using selected ion monitoring. The proposed MSPD method was applied to determine pesticide residue levels in fruit juices sold in Spanish supermarkets. At least one pesticide was found in most of the samples, although the levels detected were very low, far from the maximum residue levels established for raw fruit.

Determination of 266 pesticide residues in apple juice by matrix solid-phase dispersion and gas chromatography–mass selective detection

“…MSPD was first applied to extract and purify drug residues in animal tissue samples [14], and in recent years its application became popular in pesticide detection and has been introduced to multi-residual analysis [13][14][15][16][17][18][19][20][21] on pesticides in vegetal samples such as fruits, vegetables, fruit juices, etc.…”

Application of Rapid Resolution Liquid Chromatography to the Analysis of Some Pesticide Residues in Apple Juice

“…organophosphorus and organonitrogen) in fruits, vegetables and their juices, among which the most widely used are Gas Chromatography (GC) equipped with different detectors, such as: Mass Spectrometry (MS) (Mercer, 2005, Chua et al 2005, Cunha et al 2009, Wang et al 2006, Hu et al 2004, Flame Photometric Detector (FPD) (Tseng et al 2007), Nitrogen Phosphorous Detector (NPD) (Albero et al 2003, Attallah et al 2012, and Liquid Chromatography (LC) with Tandem Mass Spectrometry (MS/MS) (Perret et al 2002, Pang et al 2006, Borba da Cunha et al 2004, Fluorescent detector (FD) (Fillion et al 2000), etc. Although it is characterized by lower sensitivity than GC-MS and LC-MS and is not normally used for the analysis of complex samples, HPLC combined with ultraviolet (UV) and/or Diode Array Detector (DAD) is used for the determination of organophosphorus and triazines in different matrices (Rodriguez-Cuesta et al 2005, Sanchez-Ortega et al 2005, Baranowska et al 2005, Texeira et al 2004, Melo et al 2005.…”

Development and Validation of a Method for the Simultaneous Determination of 20 Organophosphorus Pesticide Residues in Corn by Accelerated Solvent Extraction and Gas Chromatography with Nitrogen Phosphorus Detection

“…Organophosphorus pesticides are usually determined by gas chromatography (GC) with flame photometric detection (FPD) [13,18], nitrogen-phosphorus detection (NPD) [14,15,21], mass spectrometry detection (MS) [16,17,[21][22][23][24][25], and liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) [23,24].…”