Multiresidue analysis of pesticides in three Indian soils: method development and validation using gas chromatography tandem mass spectrometry

Abstract

The paper reports a multiresidue method that was validated on 220 multi-class pesticides in three major Indian soils, namely, (i) new alluvial soil (NAS); (ii) red lateritic soil (RS) and (iii) black soil (BS) from three different regions. An ethyl acetate-based extraction method with a freezing-out cleanup step was employed for sample preparation, followed by gas chromatography-tandem mass spectrometric analysis. The method that was initially optimized on BS worked satisfactorily for the other two soil matrices. At the spiking level of 10 µg/kg (LOQ), the recoveries were satisfactory (within 70–120%) with precision-RSDs, ≤20% (n = 6) for 85, 88.6, and 89% of compounds in BS, RS, and NAS respectively. At 20 µg/kg, the method performance was satisfactory in each soil for all pesticides. When this validated method was applied to analyse 25 field samples, 6 pesticides were detected in them. In each case, precision (RSD) was <20%. The method sensitivity, accuracy and precision complied with the SANTE/2020/12830 guidelines. The method can be applied for environmental monitoring and risk assessment purposes, thus aiding in regulating pesticide usage in agricultural fields. The limitations and future scope of the study are also discussed.

Highlights

• A multiresidue method is reported for simultaneous analysis of multi-class pesticides in diverse soils

• The method was validated on 220 pesticides in new alluvial, red lateritic and black soils

• Sample preparation involved extraction with ethyl acetate and cleanup by a freezing step

• The residues were estimated by gas chromatography tandem mass spectrometry (GC-MS/MS)

• The method accuracy and precision complied with the EU’s SANTE guidelines

Keywords:

• Cleanup optimisation
• ethyl acetate extraction
• gas chromatography-tandem mass spectrometry
• multiresidue pesticide analysis
• soils

Acknowledgements

We are thankful to Suparna Banerjee for offering editorial support.

Disclosure statement

No potential conflict of interest was reported by the author(s).

Data availability statement

All data are available with the authors and would be made available if required.

Additional information

Funding

The author(s) reported there is no funding associated with the work featured in this article.