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Abstract: Provisional molecular weights and chemical formulas were assigned to 4 significant previously unidentified contaminants present during active fish kills in the Red River region of Oklahoma. The provisional identifications of these contaminants were determined using high‐resolution liquid chromatography–time‐of‐flight mass spectrometry (LC‐TOFMS), LC‐Fourier transform ion cyclotron resonance mass spectrometry (LC‐FTICRMS), and LC‐ion trap mass spectrometry (LC‐ITMS). Environmental water samples were extracted using a solid‐phase extraction (SPE) method, and sediment samples were extracted using a modified sonication liquid extraction method. During screening of the samples, 2 major unknown chromatographic peaks were detected at m/z 624.3 and m/z 639.3. The peak at m/z 639.3 was firmly identified, through the use of an authentic standard, as a porphyrin, specifically chlorin‐e6‐trimethyl ester, with m/z 639.31735 (M + H)+ and molecular formula C37H43N4O6. The other major peak, at m/z 624.3 (M + H)+, was identified as an amide‐containing porphyrin. It was discovered that the amide compound was an artifact created during the SPE process by reaction of ammonium hydroxide at 1 of 3 potential reaction sites on chlorin‐e6‐trimethyl ester. Other unique nontargeted chemicals were also detected and the importance of their identification is discussed. Environ Toxicol Chem 2018;37:336–344. Published 2017 Wiley Periodicals Inc. on behalf of SETAC. This article is a US government work and, as such, is in the public domain in the United States of America. [ABSTRACT FROM AUTHOR]

Abstract: Over the last 40 years, many organometallic compounds have been synthesized and used in a variety of consumer, agricultural, and industrial products. Including wastewater effluents, leaching, and direct land and water applications, there are many pathways that can disperse organometallics to the environment. Many of these compounds reach environmental compartments unchanged while others are transformed into chemical entities having different availability or toxicity to living organisms. Differences in the toxicological, biochemical, and environmental behavior of the various chemical forms of a trace element often make the determination of the total element concentration inadequate. Considerable analytical progress in organometallic speciation has been made over the past decade, when hyphenated techniques involving highly efficient separation and sensitive detection have become the techniques of choice. Methods based on liquid chromatographic separation with mass spectrometric detection have revealed new organometallic compounds in environmental and biological matrices, contributing to a better understanding of biological effects and environmental fate of organometallics. This article surveys recent applications of liquid chromatography–mass spectrometry (LC–MS) and liquid chromatography–mass spectrometry–mass spectrometry (LC–MS2) for the determination of organometallic compounds in environmental matrices. [Copyright &y& Elsevier]