[Determination of hexabromocyclododecane in coatings by gas chromatography-mass spectrometry]

A method has been developed for the determination of hexabromocyclododecane (HBCD) in fire proof coatings by gas chromatography-mass spectrometry (GC-MS). The sample was extracted with dichloromethane and purified through an organic membrane before analysis with GC-MS. The characteristic fragments (m/z 157, 239, 319, 401) and the quantitative ion (m/z 239) were selected. With the optimized conditions, the good linear relationship was obtained between the peak area and the mass concentration of HBCD in the range of 5 to 100 mg/L with the correlation coefficient more than 0. 999. The spiked recoveries in the coatings of acrylic and epoxy resins were 92.9% - 116.3% with the RSDs not more than 8%. The LOD (S/N > or = 3) of HBCD was 30 microg/g, and the LOQ (S/N > or = 10) was 100 microg/g, which were much lower than the international maximum residue limit. The method is simple, quick, accurate and precise, which can meet the requirements of the European Commission Regulation (EC) No. 1907/2006 and Norway PoHS instruction (Prohibition on Certain Hazardous Substances in Consumer Products) for the determination of HBCD. It is suitable for the analysis of HBCD in fire proof coatings.