Organotin analysis
TBT, DBT and monobutyltin (MBT) were measured in the
whole tissues of 10–15 pooled females for each station.
Butyltin compounds were extracted from 0.25 g of sample
with 5 mL of acetic acid (CH3COOH) using a microwave
system (CEMExplorer, 3 min at 40W). Tripropyltin was used
as an internal standard and was added before the microwave
irradiation procedure. A procedure blank was also performed
in the same extraction run. Butyltin species determination was
performed by standard additions, and this procedure was
applied on a pooled sample by adding an appropriate volume
of a standard solution containing TBT, DBT and MBT before
the derivatisation procedure. Derivatisation was applied as
follows: 1 mL of the supernatant was buffered to pH 4.5 with
5 mL of a 1 mol L−1 acetic acid/sodium acetate solution, and
the pHwas adjusted with ammonia. Onemilliliter of isooctane
and 1 mL of freshly prepared 1 % aqueous sodium
tetraethylborate (NaBEt4) solution were added, the mixture
shaken at 300 rpm for 20 min, and after phase separation, the
organic layer was transferred into an amber gas chromatography
(GC) autosampler vial and directly injected into the gas
chromatography–inductively coupled plasma–mass spectrometry
(GC-ICP-MS) system. All extraction and dilution
operations were performed, taking the weight with an
Organotin analysisTBT, DBT and monobutyltin (MBT) were measured in thewhole tissues of 10–15 pooled females for each station.Butyltin compounds were extracted from 0.25 g of samplewith 5 mL of acetic acid (CH3COOH) using a microwavesystem (CEMExplorer, 3 min at 40W). Tripropyltin was usedas an internal standard and was added before the microwaveirradiation procedure. A procedure blank was also performedin the same extraction run. Butyltin species determination wasperformed by standard additions, and this procedure wasapplied on a pooled sample by adding an appropriate volumeof a standard solution containing TBT, DBT and MBT beforethe derivatisation procedure. Derivatisation was applied asfollows: 1 mL of the supernatant was buffered to pH 4.5 with5 mL of a 1 mol L−1 acetic acid/sodium acetate solution, andthe pHwas adjusted with ammonia. Onemilliliter of isooctaneand 1 mL of freshly prepared 1 % aqueous sodiumtetraethylborate (NaBEt4) solution were added, the mixtureshaken at 300 rpm for 20 min, and after phase separation, theorganic layer was transferred into an amber gas chromatography(GC) autosampler vial and directly injected into the gaschromatography–inductively coupled plasma–mass spectrometry(GC-ICP-MS) system. All extraction and dilutionoperations were performed, taking the weight with an
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