A derivatization strategy for the detection and identification of volatile trialkylphosphites using liquid chromatography-online solid phase extraction and offline nuclear magnetic resonance spectroscopy

Mazumder, Avik; Gutch, P. K.; Dubey, D. K.

doi:10.1016/j.chroma.2015.03.031

Cited by 4 publications

(4 citation statements)

References 23 publications

(21 reference statements)

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“…However, these methods require clean chemical reactions, and they may not occur universally in all types of matrices or proceed to completion. The use of LC-NMR spectroscopy for sample cleanup 28 also has its own limitations . Therefore, the hydrocarbon background elimination ability of the CTF sorbent-based SPE method was explored for the 1 H NMR analysis of these analytes in the presence of hydrocarbon backgrounds containing organic matrices.…”

Section: Results and Discussionmentioning

confidence: 99%

“…The use of LC-NMR spectroscopy for sample cleanup 28 also has its own limitations. 70 Therefore, the hydrocarbon background elimination ability of the CTF sorbent-based SPE method was explored for the 1 H NMR analysis of these analytes in the presence of hydrocarbon backgrounds containing organic matrices. Each analyte (SM and HN3) was separately spiked at a concentration of 10 μg mL −1 in n-hexane containing a diesel (5000 μg mL −1 ) background and also in the dodecane (50:50 v/ v) matrix to prepare two sets of samples (two samples for each).…”

Section: Analytical Performance Of the Optimized Spementioning

confidence: 99%

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Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and ¹H NMR Analysis of Chemical Weapons Convention Related Compounds

Roy

Mazumder

et al. 2019

ACS Appl. Mater. Interfaces

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The strict monitoring and precise measurements of chemical warfare agents (CWAs) in environmental and other complex samples with high accuracy have great practical significance from the forensic and Chemical Weapons Convention (CWC) verification point of view. Therefore, this study was aimed to develop an efficient extraction and enrichment method for identification and quantification of toxic agents, especially with high sensitivity and multidetection ability in complex samples. It is the first study on solid-phase extraction (SPE) of CWAs and their related compounds from hydrocarbon backgrounds using covalent triazine-based frameworks (CTFs). This nitrogenrich CTF sorbent has shown an excellent SPE performance toward sample cleanup by selective elimination of hydrocarbon backgrounds and enrich the CWC related analytes in comparison with the conventional and other reported methods. The best enrichment of the analytes was found with the washing solvent (1 mL of n-hexane) and the extraction solvent (1 mL of dichloromethane). Under the optimized conditions, the SPE method had good linearity in the concentration range of 0.050−10.0 μg mL −1 for organophosphorus esters, 0.040− 20.0 μg mL −1 for nerve agents, and 0.200−20.0 μg mL −1 for mustards with correlation coefficients (r 2 ) between 0.9867 and 0.9998 for all analytes. Limits of detection (S/N = 3:1) in the SIM mode were found to be in the range of 0.015−0.050 μg mL −1 for organophosphorus esters, 0.010−0.030 μg mL −1 for nerve agents, and 0.050−0.100 μg mL −1 for blister agents. Limits of quantification (S/N = 10:1) were found in the range of 0.050−0.200 μg mL −1 for organophosphorus esters, 0.040−0.100 μg mL −1 for nerve agents, and 0.180−0.350 μg mL −1 for blister agents in the SIM mode. The recoveries of all analytes ranged from 87 to 100% with the relative standard deviations ranging from 1 to 8%. This method was also successfully applied for the sample preparation of 1 H NMR analysis of sulfur and nitrogen mustards in the presence of hydrocarbon backgrounds. Therefore, this SPE method provides the single sample preparation for both NMR and GC−MS analyses. KEYWORDS: triazine-based covalent organic framework, solid-phase extraction, chemical warfare agents, hydrocarbon backgrounds, organic samples, GC−MS and 1 H NMR analysis

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Section: Results and Discussionmentioning

confidence: 99%

Section: Analytical Performance Of the Optimized Spementioning

confidence: 99%

Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and ¹H NMR Analysis of Chemical Weapons Convention Related Compounds

Roy

Mazumder

et al. 2019

ACS Appl. Mater. Interfaces

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“…Therefore, absolute quantity of the analytes can be determined by mapping one (or more) of the analyte signal(s) against the area of signal(s) of some reference standard (not necessarily of the same compound). − …”

Section: Introductionmentioning

confidence: 99%

Use of Box Behnken Design for Development of High Throughput Quantitative Proton Nuclear Magnetic Resonance Experiments for Industrial Applications

Kumar

Gupta

Mazumder

et al. 2017

Ind. Eng. Chem. Res.

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The design of experiments has been used for the development of highly efficient and accurate industrial application of quantitative nuclear magnetic resonance (qNMR) spectroscopy. Since these factors are highly dependent on the choice of proper data acquisition and data processing parameters, in this work, seven data acquisition and data processing parameters (excitation pulse width/duration, central frequency, number of scans, sample temperature, acquisition time, line broadening function, and inter scan delay) were investigated and optimized for quantitative proton NMR (qHNMR) experiments to ascertain optimal values. Box Behnken design of experiments was used to arrive at these values by performing minimum number of experiments. To test this methodology, decontamination formulation number two (DS2), a universal field decontaminating reagent of highly toxic chemical warfare agents, was used as a model mixture. Quantification of its components (methyl cellosolve and diethylene triamine) was performed with respect to dimethyl sulfone (DMS) as an internal standard. Under the optimized conditions, ∼100% recovery and maximum signal-to-noise ratio (of DMS was 39908) were obtained within a short experiment time (∼15 min). Lower limits of detection and quantification for DETA were found to be 1.92 and 6.40 mg mL–1, whereas those for MC were found to be 0.89 and 2.86 mg mL–1, respectively. Finally, this method was applied for the analysis of 14 unknown samples of DS2. A t test conducted on these samples clearly indicated that there was no significant difference (p > 0.05) between the means of the results obtained from this qHNMR method and the earlier reported classical method of analysis. This clearly suggests that this novel and comprehensive methodology can be used as an independent analytical tool for quantification of the components of complex chemical mixtures.

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“…Nucleus specic observation of the analytes imparted selectivity to the NMR experiments. [57][58][59][60][61][62][63][64][65] With the use of three analytical techniques in conjunction complete decontamination of VX/ OSDEMP and concomitant formation of non-toxic products was ensured.…”

Section: Introductionmentioning

confidence: 99%

Oxidative decontamination of chemical warfare agent VX and its simulant using N,N-dichlorovaleramide

2016

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A derivatization strategy for the detection and identification of volatile trialkylphosphites using liquid chromatography-online solid phase extraction and offline nuclear magnetic resonance spectroscopy

Cited by 4 publications

References 23 publications

Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and ¹H NMR Analysis of Chemical Weapons Convention Related Compounds

Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and ¹H NMR Analysis of Chemical Weapons Convention Related Compounds

Use of Box Behnken Design for Development of High Throughput Quantitative Proton Nuclear Magnetic Resonance Experiments for Industrial Applications

Oxidative decontamination of chemical warfare agent VX and its simulant using N,N-dichlorovaleramide

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A derivatization strategy for the detection and identification of volatile trialkylphosphites using liquid chromatography-online solid phase extraction and offline nuclear magnetic resonance spectroscopy

Cited by 4 publications

References 23 publications

Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and 1H NMR Analysis of Chemical Weapons Convention Related Compounds

Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and 1H NMR Analysis of Chemical Weapons Convention Related Compounds

Use of Box Behnken Design for Development of High Throughput Quantitative Proton Nuclear Magnetic Resonance Experiments for Industrial Applications

Oxidative decontamination of chemical warfare agent VX and its simulant using N,N-dichlorovaleramide

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Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and ¹H NMR Analysis of Chemical Weapons Convention Related Compounds

Triazine-Based Covalent Organic Framework: A Promising Sorbent for Efficient Elimination of the Hydrocarbon Backgrounds of Organic Sample for GC–MS and ¹H NMR Analysis of Chemical Weapons Convention Related Compounds