GRIIDC | NO.x959.000:0018

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Petroleum source identification in marine invertebrates using gas-chromatography with tandem mass spectrometry, operated in multiple reaction monitoring mode (GC-MS/MS/MRM)

Authors: Romero, Isabel C.

Published On: Feb 25 2025 21:33 UTC

DOI: https://doi.org/10.7266/81xbk4kc

UDI: NO.x959.000:0018

Project Information

Funded By:
National Oceanic and Atmospheric Administration

Research Group:
DEEPEND/RESTORE Trends and drivers of faunal abundance of the offshore Gulf of Mexico

Point of Contact

Isabel C. Romero
University of South Florida / College of Marine Science
isabelromero@usf.edu

Data Collection Period

2011-01-10

2019-11-13

Theme keywords

oil pollution, petroleum, marine invertebrates, crude oil, marine amphipod, deep-pelagic shrimp, coastal gastropod

ISO 19115-2 Metadata

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Abstract:

The aim of this study is to fingerprint crude oil in marine invertebrates using gas-chromatography with tandem mass spectrometry, operated in multiple reaction monitoring mode (GC-MS/MS/MRM). The method was tested in a controlled microcosm laboratory experiment on the marine amphipod Corophium volutator and gastropod Hydrobia ulvae. This controlled microcosm experiment provided fingerprinting diagnostic ratios that were applied to the coastal gastropod Littoraria irrorata and the deep-pelagic shrimps Acanthephyra purpurea and Systellaspis debilis. This dataset is a result of research funded by the National Oceanic and Atmospheric Administration's RESTORE Science Program (ROR - Research Organization Registry (ROR) Search https://ror.org/0042xzm63) under award #NA19NOS4510193 to Nova Southeastern University.

Leaflet

Suggested Citation:

Romero, Isabel C.. 2025. Petroleum source identification in marine invertebrates using gas-chromatography with tandem mass spectrometry, operated in multiple reaction monitoring mode (GC-MS/MS/MRM). Distributed by: GRIIDC, Harte Research Institute, Texas A&M University–Corpus Christi. doi:10.7266/81xbk4kc

Purpose:

Fingerprinting crude oil in marine invertebrates.

Data Parameters and Units:

ng/g, dw

Methods:

Sample preparation for chemical analysis: Frozen samples (20°C) were freeze-dried before chemical analysis. Dried samples were homogenized and surrogate standards were added before extraction in an Accelerated Solvent Extraction system (ASE 200®, Dionex). ASE extraction was conducted at 120°C and 1500 psi using a solvent solution of 7:3 hexane:dichloromethane. Extracts were then concentrated under nitrogen gas to a volume of ∼100 μL. Samples were analyzed on an Agilent 7890B gas chromatograph 7010 triple quadrupole mass spectrometer. Injections (1 µl) into the multi-mode inlet in split-less mode were conducted. Inlet temperature held at 325°C. A 30m fused silica column (Rxi 5Sil MS with Integra-Guard, 30m x 0.25mm x 0.25μm, Cat# 13623-124, Restek, Bellafonte, PA, USA) was used with the following oven parameters: initial temperature 60°C, hold time 2 min; ramp 1 rate 8°C/min to 200°C, hold time 0 min; ramp 2 rate 4°C/min to 300°C, hold time 0 min, ramp 3 rate 10°C/min to 350°C, hold time 5 min. Helium was used for carrier flow at a rate of 1 ml/min and Nitrogen gas was used for collision cell gas. The transfer line between the GC oven and the MS was held at 320°C, the ion source was held at 270°C, and both quadrupoles were held at 150°C. For accuracy and precision of sample sets, the instrument was tuned daily to PFTBA (perfluorotributylamine), and samples were checked with certified standards. Sample batches were re-analyzed when replicated standards exceeded ±20% of relative standard deviation (RSD), and/or when recoveries were low.