Combined isobutoxycarbonylation andtert-butyldimethylsilylation for the GC/MS-SIM detection of alkylphenols, chlorophenols and bisphenol a in mackerel samples
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The alkylphenols, chlorophenols, and bisphenol A were determined by gas chromatography/mass spectrometry-selected ion monitoring (GC/MS-SIM) followed by two work-up methods for comparison: isobutoxycarbonyl (isoBOC) derivatization andtert-butyldimethylsilyl (TBDMS) derivatization. Eleven endocrine disrupting chemicals (EDCs) of phenols in biological samples were extracted with acetonitrile and then the acetonitrile layer underwent freezing filtration 60°C for 2 hours. Solid-phase extraction (SPE) was used with XAD-4 and subsequent conversion to isoBOC or TBDMS derivatives for sensitivity analysis with the GC/MS-SIM mode. For isoBOC derivatization and TBDMS derivatization the recoveries were 92.3~150.6% and 93.8~108.3%, the method detection limits (MDLs) of bisphenol A for SIM were 0.062 μg/kg and 0.010 μg/kg, and the SIM responses were linear with the correlation coefficient varying by 0.9755~0.9981 and 0.9908~0.9996, respectively. When these methods were applied to mackerel samples, the concentrations of the 11 phenol EDCs were below the MDL.
Key wordsEndocrine disrupting chemicals Phenol isoBOC TBDMS Freezing filtration Method detection limits GC/MS-SIM
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