Quantification of Transformation Products of Unsymmetrical Dimethylhydrazine in Water Using SPME and GC-MS
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Quantification of trace concentrations of transformation products of rocket fuel unsymmetrical dimethylhydrazine (UDMH) in water requires complex analytical instrumentation and tedious sample preparation. The goal of this research was to develop a simple and automated method for sensitive quantification of UDMH transformation products in water using headspace (HS) solid-phase microextraction (SPME) in combination with GC-MS and GC-MS/MS. HS SPME is based on extraction of analytes from a gas phase above samples by a micro polymer coating followed by a thermal desorption of analytes in a GC inlet. Extraction by 85 µm Carboxen/polydimethylsiloxane fiber at 50 °C during 60 min provides the best combination of sensitivity and precision. Tandem mass spectrometric detection with positive chemical ionization improves method accuracy and selectivity. Detection limits of twelve analytes by GC-MS/MS with chemical ionization are about 10 ng L−1. GC-MS provides similar detection limits for five studied analytes; however, the list of analytes detected by this method can be further expanded. Accuracies determined by GC-MS were in the range of 75–125% for six analytes. Compared to other available methods based on non-SPME sample preparation approaches (e.g., liquid–liquid and solid-phase extraction), the developed method is simpler, automated and provides lower detection limits. It covers more UDMH transformation products than available SPME-based methods. The list of analytes could be further expanded if new standards become available. The developed method is recommended for assessing water quality in the territories affected by space activities and other related studies.
KeywordsSPME GC-MS Quantification Transformation products Dimethylhydrazine Water
The work was conducted under the Project 0384/GF4 “Study of the impact of transportation of heptyl via the territory of Kazakhstan on the environment and habitat” funded by the Ministry of Education and Science of Kazakhstan. The experiments involving tandem mass spectrometry were performed using the instrumentation of Core Facility Center “Arktika” of Northern (Arctic) Federal University. The work was partially supported by the Russian Foundation for Basic Research (Grant 16-33-60159-mol-a-dk).
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Conflict of interest
The authors declare no conflicts of interest in relation to this research.
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