气相色谱-质谱法检测涂料中的六溴环十二烷

引用本文: 王惠, 薛秋红, 陶琳, 叶曦雯, 梁生康, 李艳秋, 牛增元. 气相色谱-质谱法检测涂料中的六溴环十二烷[J]. 色谱, 2013, 31(8): 791-794. doi: 10.3724/SP.J.1123.2013.01014 shu

Citation: WANG Hui, XUE Qiuhong, TAO Lin, YE Xiwen, LIANG Shengkang, LI Yanqiu, NIU Zengyuan. Determination of hexabromocyclododecane in coatings by gas chromatography-mass spectrometry[J]. Chinese Journal of Chromatography, 2013, 31(8): 791-794. doi: 10.3724/SP.J.1123.2013.01014 shu

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,

通讯作者: 薛秋红

基金项目:
出入境检验检疫行业标准项目(2011B052) (2011B052)

质检总局科研项目(2011IK039). (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:

English

Determination of hexabromocyclododecane in coatings by gas chromatography-mass spectrometry

1.
1. College of Chemistry and Chemical Engineering, Ocean University of China, Qingdao 266003, China;

Corresponding author: 薛秋红

Received Date: 07 January 2013
Fund Project:
出入境检验检疫行业标准项目(2011B052)

质检总局科研项目(2011IK039).

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:

gas chromatography-mass spectrometry (GC-MS)
/ hexabromocyclododecane
/ brominated flame retardants
/ coatings

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1.
沈阳化工大学材料科学与工程学院沈阳 110142

气相色谱-质谱法检测涂料中的六溴环十二烷

通讯作者: 薛秋红

English

Determination of hexabromocyclododecane in coatings by gas chromatography-mass spectrometry

Corresponding author: 薛秋红

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通讯作者: 陈斌, bchen63@163.com

中国化学会秘书处

气相色谱-质谱法检测涂料中的六溴环十二烷

通讯作者: 薛秋红

English

Determination of hexabromocyclododecane in coatings by gas chromatography-mass spectrometry

Corresponding author: 薛秋红

CCS Chemistry：嵌段共聚物自组装成 “三明治”二维有机材料，实现纳米级压力传感功能

CCS Chemistry：颜徐州、鲍哲南： 你的皮肤可能是一片SPMs

CCS Chemistry：工作高效不疲劳，只须让催化剂动起来

CCS Chemistry：静电组装导向聚合- 聚电解质纳米凝胶量化制备新策略

CCS Chemistry：金黄色葡萄球菌醛基脱氢酶是如何识别特异性底物的？

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