主题:【求助】PAH降解产物衍生化

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lanhaiqing
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多环芳烃降解产物用GC如何分析,皂化后,中性组分和酸性组分如何衍生化?
推荐答案:tjmuwyj回复于2011/10/15
PAH metabolites were derivatized
with 20 μL of N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA,
Fluke, Buchs, Switzerland). Extracts were analyzed by GC-MS to
quantify PAHs and their metabolites.

Quantification ofPAHsand Metabolites byGC-MS.

Analysis
byGC-MSwas performed with a gas chromatograph (HP-6890) coupled
to a 5973 C quadrupole mass spectrometer (Agilent Technologies,Massy,
France). The split/splitless injector was maintained at 280 C, and the
injection volume was 2 μL. The column used for separating PAHand their
metabolites was a OV-1 (Ohio-Valley) (30 m  0.25 mm inner diameter;
film thickness, 0.25 μm). The temperature gradient was 110 C (4.5min),
20 C/min until 160 C, 15 C/min until 300 C (10 min hold), and then
20 C/min until 320 C (2 min). Analyte ionization was performed by
electron ionization (70 eV), and signal acquisition was realized in the single
ion monitoring (SIM) mode. Separate analyte determination was
performed for parent PAHs and hydroxylated metabolites.
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tjmuwyj
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PAH metabolites were derivatized
with 20 μL of N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA,
Fluke, Buchs, Switzerland). Extracts were analyzed by GC-MS to
quantify PAHs and their metabolites.

Quantification ofPAHsand Metabolites byGC-MS.

Analysis
byGC-MSwas performed with a gas chromatograph (HP-6890) coupled
to a 5973 C quadrupole mass spectrometer (Agilent Technologies,Massy,
France). The split/splitless injector was maintained at 280 C, and the
injection volume was 2 μL. The column used for separating PAHand their
metabolites was a OV-1 (Ohio-Valley) (30 m  0.25 mm inner diameter;
film thickness, 0.25 μm). The temperature gradient was 110 C (4.5min),
20 C/min until 160 C, 15 C/min until 300 C (10 min hold), and then
20 C/min until 320 C (2 min). Analyte ionization was performed by
electron ionization (70 eV), and signal acquisition was realized in the single
ion monitoring (SIM) mode. Separate analyte determination was
performed for parent PAHs and hydroxylated metabolites.
tjmuwyj
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PAH metabolites were derivatized
with 20 μL of N-methyl-N-(trimethylsilyl)trifluoroacetamide (MSTFA,
Fluke, Buchs, Switzerland). Extracts were analyzed by GC-MS to
quantify PAHs and their metabolites.
LODand LOQ determined for PAHs and theirmetabolites in urine are
presented in Table 2.
Quantification ofPAHsand Metabolites byGC-MS.Analysis
byGC-MSwas performed with a gas chromatograph (HP-6890) coupled
to a 5973 C quadrupole mass spectrometer (Agilent Technologies,Massy,
France). The split/splitless injector was maintained at 280 C, and the
injection volume was 2 μL. The column used for separating PAHand their
metabolites was a OV-1 (Ohio-Valley) (30 m  0.25 mm inner diameter;
film thickness, 0.25 μm). The temperature gradient was 110 C (4.5min),
20 C/min until 160 C, 15 C/min until 300 C (10 min hold), and then
20 C/min until 320 C (2 min). Analyte ionization was performed by
electron ionization (70 eV), and signal acquisition was realized in the single
ion monitoring (SIM) mode. Separate analyte determination was
performed for parent PAHs and hydroxylated metabolites.
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