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: