Multiresidue Method for the Determination of Residues of 251 Pesticides in Fruits and Vegetables by Gas Chromatography/Mass Spectrometry and Liquid Chromatography with Fluorescence Detection

Abstract

A method is described for the determination of 251 pesticide and degradation product residues in fruit and vegetable samples. Extraction of the sample with acetonitrile is followed by a saltingout step. Co-extractives are removed by passing a portion of the acetonitrile extract through an octadecyl (C18) solid-phase extraction cleanup cartridge and then, in a second cleanup, through a carbon cartridge coupled to an amino propyl cartridge. Determination is by gas chromatography with mass-selective detection in the selected-ion monitoring mode, and by liquid chromatography with post-column reaction and fluorescence detection for N-methyl carbamates. The method has been used for analysis of various fruits and vegetables, such as apple, banana, cabbage, carrot, cucumber, lettuce, orange, pear, pepper, and pineapple. Limits of detection range between 0.02 and 1.0 mg/kg for most compounds. Over 80% of the compounds have a limit of detection of ≤0.04 mg/kg.

Residue analysis of 500 high priority pesticides: Better by GC–MS or LC–MS/MS?

“…Advantages of EI ionization are a low influence of molecular structure on response, and a large number of characteristic fragments. Extensive studies describe the simultaneous determination of 245–400 pesticides by GC–EI–MS with single quadrupole mass filters (Cairns et al, 1993; Fillion, Sauve, & Selwyn, 2000; Stan, 2000; Chu, Hu, & Yao, 2005). The use of ion traps in scan mode is more simple because no selection of characteristic ions is necessary during data acquisition.…”

“…Gas chromatography–mass spectrometry (GC–MS) has been practiced in analyzing pesticides for several decades and most characteristic ions are available from pesticide analytical manuals, applications of instrument producers, or spectral databases supplied by producers of analytical standards. In addition, some excellent articles covering GC–MS analysis of a broad range of pesticides are published (Fillion, Sauve, & Selwyn, 2000; Wong et al, 2003; Chu, Hu, & Yao, 2005). Only for some pesticides, the characteristic ions in Table 1 are obtained from recent articles or studies conducted by the pesticide industry.…”

“…The applicability of GC–MS in pesticide residue analysis is summarized in pesticide analytical manuals (Thier & Zeumer, 1992; van Zoonen, 1998), applications from instrument producers (Agilent Technologies, 1999), or scientific studies (Cairns et al, 1993; Fillion, Sauve, & Selwyn, 2000; Wong et al, 2003). Several mass spectral databases contain electron impact (EI) mass spectra of many pesticides (Ehrenstorfer, 2005; NIST/EPA/NIH, 2005).…”

A quantitative determination of fluorochloridone in rat plasma by UPLC‐MS/MS method: application to a pharmacokinetic study

“…The sample pretreatment was performed based on the previous studies with a little change (Li et al, 2012;Fillion et al, 2000). The rat plasma samples (100 μL, including calibration samples, QC samples and real samples) were added 10 μL of IS solution (verapamil, 0.05 μg/mL in methanol) and mixed for 30 s, and then 300 μL acetonitrile added for protein precipitation.…”

Application of the solid-phase micro-extraction technique coupled to GC-MS in the control of the impact of the pest treatment products in the industrial unit on the industrialized food products Quality

“…It has been demonstrated that they are particularly toxic, not only to humans but also to the environment [3][4] . These molecules tend to accumulate in different biotic and abiotic matrices, including water, air, soil, aquatic organism, blood and food [5][6][7][8][9][10][11][12][13][14][15][16][17][18] . It is noted that pesticides are among the oldest organic synthetic chemicals used in agriculture activities all over the world, since 1940, due to their energetic efficiency against pests and diseases [6][7] .…”