Application of a Pentafluorobenzyl Bromide Derivatization Method in Gas Chromatography/Mass Spectrometry of Trace Levels of Halogenated Phenols in Air, Water and Sediment Samples

Abstract

An analytical method using pentafluorobenzyl bromide (PFBB) derivatization and gas chromatography/mass spectrometry (GC/MS) has been applied to identify and quantify chloro-, bromo-and dichlorophenols in air, water and sediment samples. Phenols in air sample were collected with a PS-2 Sep-PAK TM cartridge, and eluted with 2-propanol. For water and sediment samples, liquid-liquid extraction with dichloromethane was carried out, and the solvent was exchanged to 2-propanol. The phenols in the solution reacted with PFBB to form the corresponding pentafluorobenzyl esters. After extracting the derivatives into hexane, the determination was carried out by GC/MS with selected-ion monitoring. The detection limits of phenols in air, water and sediment were 0.0033 -0.0073 µg/m 3 , 0.0066 -0.0147 µg/L and 0.33 -0.73 µg/kg, respectively. More than 90% recoveries of the halogenated phenols were obtained from real environmental samples spiked by the halogenated phenols. The three isomers of mono-chlorophenols were detected in sediment samples in the range of 5.2 -9.2 µg/kg in wet weight basis.

Determination of the [15N]-Nitrate/[14N]-Nitrate Ratio in Plant Feeding Studies by GC–MS

“…This is in accordance with the literature, where 2,3,4,5,6-pentafluorobenzyl derivatives are usually analyzed by MS after electron capture negative ion chemical ionization [93,96,97,98]. In addition, 2,3,4,5,6-pentafluorobenzyl bromide reacts also with many other compounds typically present in plants, for instance phenolics [99] and fatty acids [98]. In contrast, mesitylene gave very promising results: a peak at m / z 148 was obtained for [ 14 N]-nitrate (Figure 1B).…”

Optimization Strategy for Isocratic Separation of Halogenated Phenols by Reversed Phase Liquid Chromatography with Methanol-Water Mobile Phase

“…At the study conducted by Hanada et al 32 , 0.0033-0.0073 g was determined as the detection limit for halogenated phenols. By making use of this detection limit, in result of these studies it was determined that no halogenated phenol detection found at the chromatogram of the water sample of the lowest phase.…”

To the Question the Choice of a Derivatizing Agent for the Transfer of Methylphosphonic Acid and its O-alkils Ethers to Chromatographic Derivatives

“…Для получения летучих производных продуктов деструкции фосфорорганических соединений используются три варианта дериватизации: метилирование; третбутилдиметилсилилирование; пентафторбензилирование [5][6][7][8][9][10][11]. При трех различных способах дериватизации выдерживалось одинаковое содержание метилфосфоновой кислоты и ее эфиров в объеме пробы, равном 0,35 см 3 .…”