DETERMINATION OF EXPLOSIVE COMPOUNDS IN SOIL BY HPLC-UV METHOD USING MODIFIED QUECHERS SAMPLE PREPARATION
DOI:
https://doi.org/10.15421/jchemtech.v33i4.336927Keywords:
validation, explosives, soil, HPLC-UV, QuEChERSAbstract
The method for analyzing explosives in soil was developed by HPLC-UV employing a modified QuEChERS sample preparation technique. The method of simultaneous determination of fourteen explosives in soil was validated according to the following criteria: specificity, linearity, limits of detection (LOD), limits of quantification (LOQ), accuracy, and precision. The chromatographic conditions for separation and determination of the explosives were optimized during the study. It was established that the most optimal mobile phase for the separation of fourteen explosives is water: formic acid in a ratio of 99.9 : 0.1 (by volume; eluent A) and methanol: formic acid in a ratio of 99.9 : 0,1 (by volume; eluent B). Chromatography was performed in isocratic mode (eluent A/B, 60/40). It was found that the correlation coefficients for fourteen explosives range from 0.998 to 0.999 (R2 > 0.995). The limit of detection (LOD) and limit of quantification (LOQ) for explosives range from 0.012 to 0.081 mg/kg and 0.040 to 0.270 mg/kg, respectively. Percent recovery (R, %) in the range from 73.0 to 95.7 % indicates the acceptability of the explosives extraction procedure. The relative standard deviation (RSD, %) of the measurement results under conditions of repeatability ranged from 3.6 to 9.6 %. The obtained data suitability evaluation of method (validation) comply with the requirements of ISO 11916-1:2013 and method 8330A. The determined parameters of the proposed method also meet all the suitability assessment criteria and minimum permissible values according to Commission Decision 2002/657/EC. Therefore, the presented method is suitable for use in chemical analytical laboratories to determine the residual quantities of explosives in soils at the appropriate level.
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