Organic compounds in non-saline sediments 161
the possibility that less hydrophilic pharmaceuticals like mefenamic acid are present as
suspended particulate material, although the amounts are small in comparison with the
concentration found in aqueous phase. Additional work will be necessary to evaluate
the full importance of particle-bound pharmaceuticals with respect to transportation
in the environment.
Minton et al [203] used liquid chromatography coupled with mass spectrometry
to determine pharmaceuticals in sediments.
6.8.7 Sterols
Drier et al [204] determined sterols in lacustrine sediments. Samples of wet lacustrine
sediments were heated under anoxic conditions at 150, 175, 200 and 250
◦ C for five
days with influx of potassium hydroxide and methanol to remove sterols,and at 175
◦ C
for 12, 18, 24, and 48 hours, after which extraction was performed. Heating the
sediment increased the amounts of extractable sterols provided that the temperature
did not exceed 200
◦ C, because degradation became rapid above that temperature. The
behaviour of sterol ketones was similar, but the temperature limit was slightly higher.
The various levels of the sterols extracted are tabulated; 4-methylsterols had a high
stability towards thermal degradation under the conditions used.
Chou and Liu et al [205] determined total fecal sterols in waste water sediments
by gas chromatography-mass spectrometry.
The method included direct saponification, solvent phase extraction, derivatisation with N-methyl-N-trimethyltrifluoroacetamide and catalyst, and separation
by gas chromatography, with an HP-50
+ capillary column, followed by qualitative and quantitative analysis by mass spectrometry. Recoveries of nine sterols by
this method were 78–89%. The indicators of biopollution markers (coprostanone×
coprostanol/epicoprostanol) in different sources of wastewater effluent were calculated
as human 0.913 ± 0.251, pig 0.224 ± 0.135, cow 0.023 ± 0.001, duck 0.007 ± 0.001;
such indicators are feasible for distinguishing between different animal sources of fecal
pollution in water.
6.8.8 Miscellaneous
Che et al [207] determined synthetic musks in lake sediments using accelerated solvent
extraction followed by GCMS.
Synthetic substitutes for natural musks, are widely distributed in the environment.
They have been detected in water, sludge, fish, shrimp, mussels and other aquatic animals, and even in human’s adipose tissue, blood and breast milk. In this study Chi
et al [207] described a new extraction procedure, based on the accelerated solvent
extraction successfully coupled with gas chromatography-mass spectrometry for the
analysis of musks in sediment samples. With this method the limits of detection as low
as 0.03–0.05 ng g
−1 and the recovery rate of 86.0%–104% are achieved. When compared with Soxhlet extraction and ultrasonic extraction, accelerated solvent extraction
not only has the best extraction efficiency but also has advantage in extraction time and
solvent consumption. Eight musks, including six polycyclic musks (Tonalide (ANYN)
Galaxolide (HHCB), Phantolide (AHDI), Traseolide (ATII), Cashmeran (DPMI) and
Celestolide (ADBI)) and two nitro musks (musk xylene (MX) and musk ketone (MK))
the possibility that less hydrophilic pharmaceuticals like mefenamic acid are present as
suspended particulate material, although the amounts are small in comparison with the
concentration found in aqueous phase. Additional work will be necessary to evaluate
the full importance of particle-bound pharmaceuticals with respect to transportation
in the environment.
Minton et al [203] used liquid chromatography coupled with mass spectrometry
to determine pharmaceuticals in sediments.
6.8.7 Sterols
Drier et al [204] determined sterols in lacustrine sediments. Samples of wet lacustrine
sediments were heated under anoxic conditions at 150, 175, 200 and 250
◦ C for five
days with influx of potassium hydroxide and methanol to remove sterols,and at 175
◦ C
for 12, 18, 24, and 48 hours, after which extraction was performed. Heating the
sediment increased the amounts of extractable sterols provided that the temperature
did not exceed 200
◦ C, because degradation became rapid above that temperature. The
behaviour of sterol ketones was similar, but the temperature limit was slightly higher.
The various levels of the sterols extracted are tabulated; 4-methylsterols had a high
stability towards thermal degradation under the conditions used.
Chou and Liu et al [205] determined total fecal sterols in waste water sediments
by gas chromatography-mass spectrometry.
The method included direct saponification, solvent phase extraction, derivatisation with N-methyl-N-trimethyltrifluoroacetamide and catalyst, and separation
by gas chromatography, with an HP-50
+ capillary column, followed by qualitative and quantitative analysis by mass spectrometry. Recoveries of nine sterols by
this method were 78–89%. The indicators of biopollution markers (coprostanone×
coprostanol/epicoprostanol) in different sources of wastewater effluent were calculated
as human 0.913 ± 0.251, pig 0.224 ± 0.135, cow 0.023 ± 0.001, duck 0.007 ± 0.001;
such indicators are feasible for distinguishing between different animal sources of fecal
pollution in water.
6.8.8 Miscellaneous
Che et al [207] determined synthetic musks in lake sediments using accelerated solvent
extraction followed by GCMS.
Synthetic substitutes for natural musks, are widely distributed in the environment.
They have been detected in water, sludge, fish, shrimp, mussels and other aquatic animals, and even in human’s adipose tissue, blood and breast milk. In this study Chi
et al [207] described a new extraction procedure, based on the accelerated solvent
extraction successfully coupled with gas chromatography-mass spectrometry for the
analysis of musks in sediment samples. With this method the limits of detection as low
as 0.03–0.05 ng g
−1 and the recovery rate of 86.0%–104% are achieved. When compared with Soxhlet extraction and ultrasonic extraction, accelerated solvent extraction
not only has the best extraction efficiency but also has advantage in extraction time and
solvent consumption. Eight musks, including six polycyclic musks (Tonalide (ANYN)
Galaxolide (HHCB), Phantolide (AHDI), Traseolide (ATII), Cashmeran (DPMI) and
Celestolide (ADBI)) and two nitro musks (musk xylene (MX) and musk ketone (MK))