Figure 3 Reconstructed ion chromatogram of a calibration standard. Peak numbers correspond to the numbers listed in Table 1. Quality control and method validation
Related Figures (9)
Figure 1. In fish, the major metabolite of AP, in this case 2,4,6-trimethylphenol (2,4,6-TMP), is the glucuronide conjugate, whereas minor concentrations of the sulphate conjugate and unconjugated AP can also be detected. Following enzymatic treatment, both the glucuronated and sulphated APs are converted to the original AP. The sum of deconjugated and unconjugated AP are then derivatized and analysed by GC-MS. This section describes the preparation of fish bile samples for GC-EI-MS analysis of deconjugated AP-metabolites as their trimethylsilyl (TMS) derivatives (Figure 2). Table 3. Alkylphenol internal standard (APIS) stock solution; a mixture of six deuteratec alkylphenols, Quantitative Internal Standards, dissolved in methyl tert-butyl ether (Chiron Trondheim, Norway). The concentrations in the table might not be accurate, but the relative concentration should be approximately as indicated in the table. Table 4. GC-MS performance internal standard (AP-GCIS) stock solution. Remarks Table 5. List of alkylphenols (AP target), internal standards (APIS), and GC performance standard (AP-GCIS). m/z = mass/charge (for precursor ions). Oven temperature programme Total time: 40:17 min. Solvent cut time: 7.0 min GC-MS acquisition windows for determination of alkylphenols, showing which ions are determined in which time-window. (See also Jonsson et al., 2008a.) 4.7 Calculation