Determination of Pesticides in Soil by Mechanical Stirring-Assisted Extraction Coupled with Gas Chromatography-Mass Spectrometry

Abstract

This work describes the development of an analytical method for determining the mobility of some organophosphorus and azole group pesticides. The chromatographic and mass spectrophotometric parameters were optimized. The target pesticides were recovered quantitatively (79.3–95.6%) with a relative standard deviation less than 8.5% at the optimum conditions of the extraction. The limits of detection of the target pesticides were found to be in the range of 0.16 to 1 . 14  µ g   kg ^{− 1} with a correlation coefficient ( r) >  0 . 9955 . The method was validated in the target environmental matrices by the analysis of a spiked soil sample. The proposed method was successfully applied for the determination of pesticides in vineyard soil samples and statistically evaluated.

Keywords:

• Fungicide
• GC–MS
• Herbicide
• Mechanical stirring-assisted extraction (MSAE)
• Soil

Notes

^a Internal Standard. ^b  R.A.: relative abundance. ^c Quantification ions(underline indicates spectrum base peak and boldface indicates molecular mass peak).

^aµg/L. PSWE; Pressurized Subcritical Water Extraction. MAME; Microwave Assisted Micellar Extraction. HLLME; Homogeneous Liquid–Liquid Extraction. SBWE; Subcritical Water Extraction. LDMHLLE; Low Density Miniaturized Homogenous Liquid–Liquid Extraction. MSAE; Mechanical Stirring Assisted Extraction. LC-ESI-MS; Liquid Chromatography–Electrospray onization-Mass Spectrometry. HAc; Acetic acid.

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