Development of a microextraction by packed sorbent with gas chromatography‐mass spectrometry method for quantification of nitroexplosives in aqueous and fluidic biological samples

Abstract

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 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 > 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.

Current trends on microextraction by packed sorbent – fundamentals, application fields, innovative improvements and future applications

“…1 This was also previously shown for different antiepileptic drugs, 169,170 or NSAIDs. 171 In this section, however, we will mainly focus on the comparisons in recent reports involving microextraction techniques, such as DLLME, 126,172,173 HF-LPME, 87,100 SDME, 109,174 µSPE [175][176][177][178][179][180] and SPME, 1,109,133,181,182 that already incorporate significant technological improvements by comparison with more conventional techniques, such as LLE 1,87,183 and SPE (Table 5). 1,87,109,120,183 These comparisons of MEPS applications with other extraction approaches would be more meaningful if the same experimental conditions were involved but unfortunately this is not available so far for many applications.…”

Amino Monolayer Modified Nanowire Array for Trinitrotoluene Detection

“…Currently, besides off-site chemical analysis, there also exist various analytical techniques for the analysis of explosives in situ, such as gas chromatography/mass spectrometry (GC/MS), (1,2) fluorescence, (3)(4)(5) Raman spectrometry, (6,7) and ion mobility spectrometry. (8) All of these methods exhibit high capability, but are often bulky, expensive, and time-consuming.…”