摘要
建立了固相微萃取/气相色谱-质谱联用法（SPME/GC-MS）测定橡胶密封材料中N-亚硝基-N-甲基苯胺（NMPh A）、N-亚硝基-N-乙基苯胺（NEPh A）和N-亚硝基二苯基胺（NDPhe A）3种N-亚硝胺化合物含量的方法。样品参考国标GB/T 24153-2009进行预处理后,采用固相微萃取进行提取,对影响固相微萃取效率的纤维涂覆种类、萃取时间、搅拌速度和萃取温度等条件进行优化。在优化条件下,方法的线性范围为5~500μg/L,相关系数（r）均大于0.99,检出限为0.5μg/kg,回收率为77%~92%,相对标准偏差（RSD,n=6）为3.8%~7.7%。
A solid-phase microextraction（ SPME） coupled with gas chromatography- mass spectrometry was developed for the determination of N-nitroso-N-methylaniline（ NMPh A）,N-nitroso-N-ethylamine（ NEPh A） and N-nitrosodiphenylamine（ NDPhe A） in rubber sealing material. The samples were pretreated by GB / T 24153- 2009 standard method,and then extracted by SPME. Influences of fibers species,extraction time,mixing speed and temperature on extraction efficiencies of three N-nitrosamines were optimized. Under the optimized experimental conditions, the linear ranges of NMPh A,NEPh A and NDPhe A were between 5 μg / L and 500 μg / L with correlation coefficients（ r）larger than 0. 99. The method detection limits were 0. 5 μg / kg. The average recoveries were in the range of 77%- 92% with relative standard deviations（ RSD,n = 6） of 3. 8%- 7. 7%.
出处
《分析测试学报》
CAS
CSCD
北大核心
2016年第2期245-248,共4页
Journal of Instrumental Analysis
基金
国家质检总局科技计划项目(2013QK283)
关键词
橡胶密封材料
固相微萃取
气相色谱-质谱法
N-亚硝胺
rubber sealing material
solid-phase microextraction
gas chromatography-mass spectrometry
N-nitrosamine
