Determination of tributyltin (TBT) in marine sediment using pressurised liquid extraction–gas chromatography–isotope dilution mass spectrometry (PLE–GC–IDMS) with a hexane–tropolone mixture

Abstract

Extraction conditions for the determination of tributyltin (TBT) in sediment samples have been developed further. The analytical procedure is based on spiking with isotopically labelled analyte, pressurised liquid extraction (PLE) with a hexane/tropolone mixture, Grignard derivatization and quantification by GC-MS. It was applied to two unknown sediment samples as part of an intercomparison exercise of the Comité Consultatif pour la Quantité de Matière (CCQM). The detection limit was approximately 1.5 ng/g TBT as Sn, while the repeatability and intermediate precision (as the coefficient of variation) were 1.9% and 3.2%, respectively. The expanded uncertainty was 6.2% (coverage factor k = 2), and the accuracy was confirmed by measurement of a certified reference material.

Deep eutectic liquid organic salt as a new solvent for liquid-phase microextraction and its application in ligandless extraction and preconcentraion of lead and cadmium in edible oils

“…The uncertainty of results was calculated according to Guide to the Expression of Uncertainty in Measurement (GUM) [41]. Expanded uncertainty was determined using following equation [40,42,43]. Where U is the expanded uncertainty, k is the coverage factor (for the confidence limit at 95% level, k is chosen to be 2), u r(sample) is the uncertainty associated with mass of the sample, u r(cal) is the relative uncertainty associated with calibration, u r(true) is the uncertainty associated with recovery determination, u r(rep) is the uncertainty of precision, u r(LOD) is the uncertainty associated with LOD determination, c det is the mean concentration of the target analyte, SD xy is the residual standard deviation, p is the number of repetitions carried out for given sample, m is the total number of standard samples used for plotting the calibration curve, X sample is the concentration of sample, X m is the average of all the concentration of a standard solution for which the measurement was made in order to plot a calibration curve, X i is the concentration of standard solution and b is the slope of the calibration curve.…”

Trends in the analysis and monitoring of organotins in the aquatic environment

“…Microwave assisted extraction (MAE) and accelerated sample extraction (ASE) (also known as pressurised liquid extraction) are more prevalent methods, providing benefits of autonomous rapid extraction times, high sample throughput and often reduced solvent consumption [35]. SPE is used widely owing to its general availability, often yielding a higher pre-concentration factor relative to the other conventional techniques [36].…”

Maritime pollutants in shipping and commercial European ports based on relevant physical and biogeochemical environmental parameters (IUPAC Technical Report)

“…It affects negatively various invertebrates (leading to sterility or even death) [58] and it is accumulated in fish, dolphins, seals whales and other sea mammals. TBT in sediment samples can be determined by GC-MS after treatment with a solution of acetic acid/methanol with ultrasonic shredder [59]; GC-MS after spiking with isotopically labelled analyte, pressurized liquid extraction and Grignard derivatization [60]; GC-ICP-MS after treatment with a species-specific isotope dilution method [61]; a rapid and precise method performed by species specific IDMS analysis using a CGC-ICP-MS [62]; a liquid chromatographic method with fluorimetric detection using fisetin as fluorogenic reagent [63].…”