Liquid Chromatographic Determination of 1,3,5-Trinitroperhydro-1,3,5-triazine and 2,4,6-Trinitrotoluene in Human Plasma and Groundwater Samples Utilizing Microextraction in Packed Syringe

Abstract

A rapid and efficient analytical method suitable for the simultaneous determination of 1,3,5-trinitroperhydro-1,3,5-triazine (RDX) and 2,4,6-trinitrotoluene (TNT) in groundwater and human plasma samples using liquid chromatography with UV detection (LC-UV) has been developed. RDX and TNT were baseline separated within time span of 4.8 min on a reverse phase C 18 analytical column with water acetonitrile mixture in ratio 30:70 (v/v) as mobile phase. The UV detection was carried out at 234 nm. A sample preparation method for biological and environmental matrices using microextraction by packed sorbent (MEPS) technique has been implemented, employing 4 mg of C 18 silica sorbent inserted into a microvolume syringe and using only 30 lL of plasma and groundwater samples. Several factors affecting the performance of MEPS, such as number of extraction cycles, washing solvent volume, elution solvent volume and carryover etc., were optimized. Limits of detection were 0.0997 and 0.0628 ng mL -1 for RDX and TNT, respectively. The extraction yields were satisfactory for both analytes ([81.2 %) as well as the precision data, which were always in the low percentage of relative standard deviation values (\5.6 % , n = 6). The present method is miniaturized, fully automated, and robust which can be easily used for forensic studies of explosives in environmental and biological samples.

Simultaneous Determination of RDX and HMX in Rat Plasma by LC-MS/MS and its Applications

“…As the previous studies reported, the quantitative detection ranges of RDX were 1.00-500.00 ng•ml −1 (Bansal et al, 2012) and 10.00-2000.00 ng•ml −1 (Özhan et al, 2003). Compared with previous studies, the quantitative detection scope of this study is narrow, but the LOD is the lowest.…”

“…Their wide usages often lead to the uncontrolled discharge of RDX and HMX into the environment. RDX and HMX are moderately to slightly soluble in water, and thus can migrate through groundwater ( Bansal et al, 2012 ) to cause animals ( Bannon et al, 2009 ; Gust et al, 2009 ; Williams et al, 2012 ; Kuperman et al, 2013 ), plants ( Vila et al, 2007 ) and humans ( Johnson et al, 2007 ) contamination. In addition, they can also adversely affect mammals through inhalation or oral and dermal exposure ( Talmage et al, 1999 ).…”

“…Therefore, quantitative detection original form of RDX and HMX in vivo is a good method for the treatment and early warning of poisoning. But the currently accepted analytical methods for the determination of nitramines in biological fluids are limited ( Woody et al, 1986 ; Özhan et al, 2003 ; Bansal et al, 2012 ). Liquid chromatography combined with UV detection was chosen for these studies and the limited detections were circumscribed.…”

Simultaneous determination of multiple components in explosives using ultraviolet spectrophotometry and a partial least squares method

“…The most common methods involve ion mobility spectrometry (IMS), [9][10][11][12] mass spectrometry (MS), [13][14][15] Raman spectroscopy, 5,16,17 THz spectroscopy, [18][19][20] laser induced breakdown spectroscopy (LIBS), 21-24 gas chromatography (GC), [25][26][27] high performance liquid chromatography (HPLC) [28][29][30][31] and some combined methods (viz. The most common methods involve ion mobility spectrometry (IMS), [9][10][11][12] mass spectrometry (MS), [13][14][15] Raman spectroscopy, 5,16,17 THz spectroscopy, [18][19][20] laser induced breakdown spectroscopy (LIBS), 21-24 gas chromatography (GC), [25][26][27] high performance liquid chromatography (HPLC) [28][29][30][31] and some combined methods (viz.…”

Preparation and Characteristics of Rat Anti-1,3,5-Trinitroperhydro-1,3,5-Triazine (RDX) Monoclonal Antibody and Detection of RDX Using Surface Plasmon Resonance Immunosensor

“…They include (1) the detection of explosives attached on a surface using lasers [8], (2) the detection of explosives using optical fibers [9], [10], (3) incorporating π-π interaction into an SPR immunosensor [11], and (4) the detec- tion of explosives based on antigen-antibody interactions of antigen analogues or antibodies that are fluorescently labeled or labeled with a dye [12]- [14]. Some papers reported the extraction and detection of RDX from real samples, such as groundwater and plasma [15]. However, practical applications of the methods previously reported seem difficult to realize, considering the various sites where the explosive sensors will be actually used, in terms of sensitivity, selectivity, measurement time, and cost.…”