Analytical Sciences

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

Yoshifumi HANADA,*¹ Iwao IMAIZUMI,*² Kozo KIDO,*¹ Teizi TANIZAKI,*¹ Minoru KOGA,*³ Hiroaki SHIRAISHI,*⁴ and Mitsuyuki SOMA*⁵

*1 Kitakyushu City Institute of Environmental Sciences, Shin-ike 1-2-1, Tobata, Kitakyushu 804-0082, Japan
*2 Environment Bureau of Kitakyushu City Office, Zyonai 1-1, Kokura-kita, Kitakyushu 803-8501, Japan
*3 Prefectural University of Kumamoto, Tukide 3-1-100, Kumamoto 862-8502, Japan
*4 The National Institute for Environmental Studies, Onogawa, Tsukuba, Ibaraki 305-0053, Japan
*5 University of Shizuoka, Yada 52-1, Shizuoka 422-8526, Japan

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 ug/m³, 0.0066 - 0.0147 ug/L and 0.33 - 0.73 ug/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 ug/kg in wet weight basis.

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