Single drop microextraction and gas chromatography–mass spectrometry for the determination of diflufenican, mepanipyrim, fipronil, and pretilachlor in water samples

Abstract

An analytical method for the determination of diflufenican, mepanipyrim, pretilachlor, and fipronil in water samples was developed using single drop microextraction in the direct immersion mode and gas chromatography-mass spectrometry. A factorial fractionated design of type 2(6-1) at two levels was performed, to study the influence of experimental variables such as ionic strength, pH, agitation speed, extraction time, drop volume, and sample volume. To establish the optimal conditions for the variables that were significant, a Doehlert design was performed. The optimum conditions of extraction were 1 μL of heptane immersed in 4.0 mL of sample with continuous agitation at 500 rpm for 30 min at room temperature. The developed method proved to have good linearity for the range studied. The detection limits were 0.07 μg L(-1) for diflufenican, 0.03 μg L(-1) for mepanipyrim, 0.08 μg L(-1) for pretilachlor, and 1.39 μg L(-1) for fipronil. The method was validated on river water samples, showing the absence of matrix effect and recoveries ranged from 90.1 to 107.8 %. The results show that the method developed is accurate, sensitive, rapid, simple, and low cost, so it is recommended for application in the analysis of these different classes of pesticides in water samples.

Ultimate fate, transformation, and toxicological consequences of herbicide pretilachlor to biotic components and associated environment: An overview

“…Sha‐Sha et al (2013) proposed magnetic solid‐phase extraction (MSPE) comprising graphene nanocomposite (G‐Fe 3 O 4 ) as the adsorbent, coupled with dispersive liquid–liquid microextraction (DLLME) using GC‐FID to detect five chloroacetanilide herbicides including pretilachlor from water and tea infusions with LOD of 0.03 μg/L. Another simple and cost‐effective analytical method using SDME with GC‐MS was developed to determine pretilachlor in water samples with LOD of 0.08 μg/L (Araujo et al, 2013). Similarly, Li et al (2013) reported pretilachlor detection using MSPE and GC‐ECD with LOD of 0.05 μg/L.…”

Label-Free Aptasensor for Detection of Fipronil Based on Black Phosphorus Nanosheets

“…Headaches, dizziness, sweating, and other symptoms have been described because of fipronil poisoning in humans [ 7 ]. Currently, the most common techniques for detecting fipronil are gas chromatography-mass spectrometry (GC-MS), liquid chromatography-mass spectrometry (LC-MS), and gas chromatography (GC) [ 8 , 9 , 10 ]. However, these traditional methods have challenges, such as complex sample pretreatment, high cost, and dependence on trained staff.…”

Development of a direct competitive enzyme-linked immunosorbent assay for determination of the fungicide mepanipyrim and its metabolite

“…5) Mepanipyrim residue is generally detected by using a chromatography technique, such as high-performance liquid chromatography (HPLC) with a diode array detector, liquid chromatography with tandem mass spectrometry, or gas chromatography with mass spectrometry. 6,7) The instruments used in these techniques are sensitive, accurate, and suitable for the multi-residue analysis of pesticides containing mepanipyrim. On the other hand, when detecting only mepanipyrim is the objective, enzyme-linked immunosorbent assays (ELISAs) are also useful methods.…”