气相色谱-质谱法检测涂料中的六溴环十二烷  

Determination of hexabromocyclododecane in coatings by gas chromatography-mass spectrometry

作　　者：王惠[1,2] 薛秋红[2] 陶琳[3] 叶曦雯[2] 梁生康[1] 李艳秋[2] 牛增元[2] 

机构地区：[1]中国海洋大学化学化工学院,山东青岛266003 [2]山东出入境检验检疫局,山东青岛266000 [3]淄博出入境检验检疫局,山东淄博255000

出　　处：《色谱》2013年第8期791-794,共4页Chinese Journal of Chromatography

基　　金：出入境检验检疫行业标准项目(2011B052);质检总局科研项目(2011IK039)

摘　　要：建立了防火涂料中阻燃剂六溴环十二烷(HBCD)的气相色谱-质谱(GC-MS)分析方法。样品用二氯甲烷进行萃取,萃取液经有机滤膜过滤后,用气相色谱-质谱联用仪进行测定。在选择离子检测模式下以m/z 157、239、319、401为定性离子,m/z 239为定量离子进行结构确证和定量检测。在优化的实验条件下,六溴环十二烷标准溶液在5～100 mg/L的质量浓度范围内线性关系良好,相关系数大于0.999。对市售的空白丙烯酸树脂涂料样品及环氧树脂涂料样品进行加标回收试验,结果表明本方法的平均回收率为92.9%～116.3%,RSD不超过8%。方法的检出限(S/N=3)为30μg/g,定量限(S/N=10)为100μg/g。本方法简便、快速、准确性好、精密度高,能够满足检测工作的实际要求。A method has been developed for the determination of hexabromocyclododecane （HBCD） in fire proof coatings by gas chromatography-mass spectrometry （GC-MS）. The sam- ple was extracted with dichloromethane and purified through an organic membrane before anal- ysis 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≥3） of HBCD was 30 μg/g, and the LOQ （S/N≥10） was 100 μg/g, which were much lower than the international maximum residue limit. The method is simple, quick, accurate and pre- cise, which can meet the requirements of the European Commission Regulation （EC） No. 1907/2005 and Norway Polls instruction （Prohibition on Certain Hazardous Substances in Con- sumer Products） for the determination of HBCD. It is suitable for the analysis of HBCD in fire proof coatings.

关 键 词：气相色谱-质谱法 六溴环十二烷 含溴阻燃剂 涂料 

分 类 号：O658[理学—分析化学]