Gas chromatography/mass spectrometry comprehensive analysis of organophosphorus, brominated flame retardants, by-products and formulation intermediates in water.

A multiresidue method based on gas chromatography coupled to quadrupole mass spectrometry was developed to determine organophosphorus flame retardants, polybromodiphenyl ethers (BDEs 28, 47, 99, 100, 153, 154, 183 and 209), new brominated flame retardants, bromophenols, bromoanilines, bromotoluenes and bromoanisoles in water. Two ionization techniques (electron ionization--EI, and electron capture negative ionization--ECNI) and two acquisition modes (selected ion monitoring--SIM, and selected reaction monitoring--SRM) were compared as regards to mass spectral characterization, sensitivity and quantification capabilities. The highest sensitivity, at expenses of identification capacity, was obtained by GC-ECNI-MS/SIM for most of the compounds analyzed, mainly for PBDEs and decabromodiphenyl ethane while GC-EI-MS/MS in SRM was the most selective technique and permitted the identification of target compounds at the pg level, and identification capabilities increased when real samples were analyzed.

Fingerprinting of Cretaceous higher plant resins by infrared spectroscopy and gas chromatography coupled to mass spectrometry.

Ambers from Peñacerrada (Basque Country, North Spain) have been analysed by IR spectroscopy and GC-MS in order to study the polymeric and solvent-soluble GC-amenable fractions, respectively. All samples showed branched monoalkybenzenes, bicyclic sesquiterpenoids and tricyclic diterpenoids related to pimaric acids precursors, suggesting a paleobotanic origin from araucarian species. Molecules containing oxygenated polar functionalities were not found, which is in agreement with the Cretaceous origin of the samples and in good correspondence with the IR spectra and with the low oxygen content estimated from elemental composition analysis.

Identification and quantification of n-octyl esters of alkanoic and hexanedioic acids and phthalates as urban wastewater markers in biota and sediments from estuarine areas.

A gas chromatographic method for the identification and quantification of n-octyl esters (from n-octyl tetradecanoate to n-octyl hexa-cosanoate including dioctyl hexanedioate) and phthalates [dibutyl phthalate, benzyl butyl phthalate and di(2-ethylhexyl) phthalate] in sediments and biota from estuarine environments is described. Standards used for identification and quantification of some n-octyl esters were synthesized. The method has allowed the analysis of these compounds in polychaeta (Nereis diversicolor), oysters (Crassostea angulata), crabs (Carcinus maenas) and fish (Chelon labrosus, Platichtys flesus and Chondostroma polylepis) that were collected at different locations of the Urdaibai estuary (Bizkaia, Basque Country, Spain).