Selective and Sensitive Quantification of Acetochlor and S-Metolachlor in Maize and Soybean Plant Samples by Gas Chromatography-Tandem Mass Spectrometry

Abstract

Herbicide residue analysis has gained importance worldwide, mainly for food quality control to minimize potentially adverse impacts on human health. A Gas chromatography-tandem mass spectrometry (GC-MS) method for quantitative analysis of acetochlor and s-metolachlor in maize and soybean straw has been developed, validated and applied to analyze the residues of anilide herbicides. Straw material was dried, homogenized and extracted with a mixture of n-hexane and acetone by an accelerated solvent extraction method. Chromatographic separation of the target analytes was performed on an Agilent 7832 GC equipped with a mass spectrometer detector, a split-splitless injector and an HP-5 MS (5% phenylmethyl siloxane) capillary column (30 m × 0.25 mm × 0.25 µm). Under these parameters, the limit of detection (LOD) values were 0.2 ng g−1 for acetochlor and 0.07 ng g−1 for s-metolachlor, with average recoveries between 86% and 119.7%. The method was validated for acetochlor and s-metolachlor in maize and soybean straw at 0.5 and 0.01 mg kg −1. Furthermore, the final residues of the two herbicides in maize and soybean straw were below the maximum residue limit (MRL) at harvest time. The proposed method is suitable for routine analysis.

Screening of 258 Pesticide Residues in Silage Using Modified QuEChERS with Liquid- and Gas Chromatography-Quadrupole/Orbitrap Mass Spectrometry

“…To define the SDL, according to SANTE/11312/2021 [26], this was the lowest level at which pesticide had been screened in at least 95% of the samples. Calibration curves were investigated by determining the results of a series of standard addition recovery experiments (1,2,5,10,20,50,100,200,300, and 500 µg kg −1 ) of blank matrix extract solutions before injection. Matrix effects were calculated using the following formula: matrix effect (ME, %) = [(slope of matrix matching standard curve-the slope of solvent standard curve)/slope of solvent standard curve] × 100.…”

“…It is vital to apply sensitive and reliable techniques to detect pesticide residues in forage. The current analytical methods for the detection of multi-pesticide residues are mainly GC-MS [19], GC-MS/MS [19,20], and LC-MS/MS [19,21]. These chromatographymass spectrometry techniques have become an essential analytical tool.…”

Flow injection chemiluminescence determination of acetochlor and cartap‐HCl in freshwater samples using an acidic KMnO4–rhodamine‐B reaction system

“…samples and formulations using different cleanup and extraction techniques [solvent extraction (SE), liquid extraction (LE), solid‐phase extraction (SPE), microextraction and quick, easy, cheap, effective, rugged and safe (QuEChERS)]. These analytical techniques include gas chromatography–electron capture detection (GC‐ECD) [12, 13], GC–tandem mass spectrometry (GC‐MS/MS) [14, 15], GC‐MS [16–19], liquid chromatography–MS/MS (LC‐MS/MS) [20–22], high‐performance liquid chromatographic‐ultraviolet (HPLC‐UV) [23, 24], ultra‐high‐performance liquid chromatography–MS/MS (UPLC‐MS/MS) [25], immunoaffinity chromatography (IAC) [26], fluorescence polarization immunoassay (FPIA) [27, 28], multiplex immunosensor [29], enzyme‐linked immunosorbent assay (ELISA) [30], piezoelectric biosensor [31], photoelectrochemical (PEC) sensor [32, 33], and flow injection spectrophotometry (FI‐Spec.) [34].…”

“…Various analytical methodologies have been devised for acetochlor estimation in environmental (air, soil, and water) and food (vegetables, fruits, etc.) samples and formulations using different analytical techniques include gas chromatography-electron capture detection (GC-ECD) [12,13], GC-tandem mass spectrometry (GC-MS/MS) [14,15], GC-MS [16][17][18][19], liquid chromatography-MS/MS (LC-MS/MS) [20][21][22], high-performance liquid chromatographic-ultraviolet (HPLC-UV) [23,24], ultra-highperformance liquid chromatography-MS/MS (UPLC-MS/MS) [25],…”

Efects of a S-Metolachlor Based Herbicide on Two Plant Models: Zea Mays L. And <i>Lactuca Sativa L.</i>

“…This herbicide acts by inhibiting various biological processes in the meristematic zones of plants. It is absorbed by the roots and aerial portions of germinating plants, and translocated via xylem to developing areas [8,9]. Once there it inhibits the synthesis of chlorophyll, proteins, fatty acids and lipids, preventing cell growth and division, and, consequently, blocking the growth of weeds soon after germination [8].…”