Combined isobutoxycarbonylation and tert-butyldimethylsilylation for the GC/MS-SIM detection of alkylphenols, chlorophenols and bisphenol A in mackerel samples.
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 and tert-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 degrees 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 approximately 150.6% and 93.8-108.3%, the method detection limits (MDLs) of bisphenol A for SIM were 0.062 microg/kg and 0.010 microg/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.
Kim
Hyub
H
Technology Innovation Center, Sangju National University, Sangju 742-711, Korea. khlyj@sangju.ac.kr
Hong
Jong-Ki
JK
Kim
Yong-Hwa
YH
Kim
Kyoung-Rae
KR
D000447:Aldehydes / Q000737:chemistry*; D000478:Alkylation; D000818:Animals; D001559:Benzhydryl Compounds; D002733:Chlorophenols / Q000032:analysis*; D004703:Endocrine System / Q000187:drug effects / Q000378:metabolism; D004784:Environmental Monitoring / Q000379:methods; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D007723:Korea; D010473:Perciformes / Q000378:metabolism*; D010636:Phenols / Q000032:analysis*; D012821:Silanes / Q000737:chemistry*; D014874:Water Pollutants, Chemical / Q000009:adverse effects / Q000032:analysis; D000098826:Bisphenol A Compounds
D000447:Aldehydes; D001559:Benzhydryl Compounds; D002733:Chlorophenols; D010636:Phenols; D012821:Silanes; D014874:Water Pollutants, Chemical; C103256:tert-butyldimethylsilane; C006780:bisphenol A; D000098826:Bisphenol A Compounds