220
content (extractable with n-hcxanc/acctonc) was determined gravimetrically. To remove
lipids from the sample, the extracts were cleaned by gel permeation chromatography
(GPC; Biobeads, column: r = 2 cm; h = 14 cm; p = 2 bar, flow = 4 mL/min). After
solvent change to hexane, the extracts were cleaned up on neutral aluminium oxide
(Merck, Darmstadt; heated for 5 h at 500°C, desactivated with 19 % w/w water).
Elution was done with hexane/dichloromethane (50/50 v/v) and pure dichloromethane.
The solvent of both fractions was changed to n-hexane, and D6-Chlorpyrifos-methyl
was added as recovery standard. The first fraction contained all target compounds. It
was concentrated to 300 pi and analysed by GC-MS (see 6.6.2).
6.6.6 Procedure for the analysis of Pentachlorophenol and
Trichloropyridinol in water
Sea water samples were taken using a 10 L sampler (glass bowl) and were acidified
with 25 % hydrochloric acid (p. a.) to pH 2.5-3.0. 13 C-pentachlorophenol was added as
internal standard. The sample was pumped through a column filled with 2 g Chromafix
HR-P resin (Macherey and Nagel) in a custom made extraction system. After drying in
a gentle nitrogen stream, the loaded columns were stored in the dark at 8°C until
elution. PCP and TCPy were eluted with methanol (100 mL). The solvent volume was
reduced to 300 pL and the extract analysed by HPLC-MS.
6.6.6.1 HPLC-MS analysis
A combination of an Agilent 1100 HPLC system and a SCIEX API 2000 triple
quadropole MS was used for HPLC-MS analysis; the parameters were as follows:
Column: Synergi 4 p Hydro-RP (Phenomenex; C18 phase with
polar endcapping) 75 x 2.00 mm
Agilent 1100
HPLC system: