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Development of a microextraction by packed sorbent with gas chromatography‐mass spectrometry method for quantification of nitroexplosives in aqueous and fluidic biological samples
Author(s) -
Dhingra Gaurav,
Bansal Pooja,
Dhingra Nidhi,
Rani Susheela,
Malik Ashok Kumar
Publication year - 2018
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.201700470
Subject(s) - chromatography , sorbent , chemistry , elution , mass spectrometry , extraction (chemistry) , detection limit , analyte , gas chromatography , gas chromatography–mass spectrometry , solvent , sample preparation , aqueous solution , solid phase microextraction , trinitrotoluene , adsorption , organic chemistry , explosive material
A new method for quantification of 12 nitroaromatic compounds including 2,4,6‐trinitrotoluene, its metabolites and 2,4,6‐trinitrophenyl‐ N ‐methylnitramine with microextraction by packed sorbent followed by gas chromatography and mass spectrometric detection in environmental and biological samples is developed. The microextraction device employs 4 mg of C 18 silica sorbent inserted into a microvolume syringe for sample preparation. Several parameters capable of influencing the microextraction procedure, namely, number of extraction cycles, washing solvent, volume of washing solvent, elution solvent, volume of eluting solvent and pH of matrix, were optimized. The developed method produced satisfactory results with excellent values of coefficient of determination (R 2 > 0.9804) within the established calibration range. The extraction yields were satisfactory for all analytes (> 89.32%) for aqueous samples and (> 87.45%) for fluidic biological samples. The limits of detection values lie in the range 14–828 pg/mL.