色谱

色谱 ›› 2013, Vol. 31 ›› Issue (8): 791-794.DOI: 10.3724/SP.J.1123.2013.01014

• 技术与应用 • 上一篇    下一篇

气相色谱-质谱法检测涂料中的六溴环十二烷

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   

  1. 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
  • 收稿日期:2013-01-07 修回日期:2013-02-11 出版日期:2013-08-28 发布日期:2013-09-29
  • 通讯作者: 薛秋红
  • 基金资助:

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

Determination of hexabromocyclododecane in coatings by gas chromatography-mass spectrometry

WANG Hui1,2, XUE Qiuhong2, TAO Lin3, YE Xiwen2, LIANG Shengkang1, LI Yanqiu2, NIU Zengyuan2   

  1. 1. College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003, China;
    2. Shandong Entry-Exit Inspection and Quarantine Bureau, Qingdao 266000, China;
    3. Zibo Entry-Exit Inspection and Quarantine Bureau, Zibo 255000, China
  • Received:2013-01-07 Revised:2013-02-11 Online:2013-08-28 Published:2013-09-29
  • Contact: O658

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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30 μg/g,定量限(S/N=10)为100 μg/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。

关键词: 含溴阻燃剂, 六溴环十二烷, 气相色谱-质谱法, 涂料

Abstract:

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≥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 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.

Key words: brominated flame retardants, coatings, gas chromatography-mass spectrometry (GC-MS), hexabromocyclododecane

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