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    固相微萃取-气相色谱-质谱法测定橡胶密封圈中8种N-亚硝胺含量

    GC-MS Determination of 8 N-Nitrosamines in Rubber Sealing Ring with Solid Phase Microextraction

    • 摘要: 采用固相微萃取-气相色谱-质谱法测定橡胶密封圈中8种N-亚硝胺的含量。按国家标准GB/T 24153-2009进行样品的预处理,然后用二乙烯基苯/聚二甲基硅氧烷萃取头,在30 ℃和800 r·min-1转速的条件下萃取45 min。在气相色谱分离中用Agilent 1701色谱柱为固定相;在质谱测定中采用选择离子监测模式。8种N-亚硝胺的线性范围均为0.10~2.0 mg·L-1,方法的检出限(3S/N)均为0.03 mg·kg-1。以空白样品为基体进行加标回收试验,回收率在73.0%~96.1%之间,测定值的相对标准偏差(n=6)在1.3%~9.7%之间。

       

      Abstract: GC-MS was applied to the determination of 8 N-nitrosamines in rubber sealing ring with solid phase microextraction. The sample was pretreated according to the standard method of GB/T 24153-2009, and then extracted for 45 min by DVB/PDMS micro-extractor at 30 ℃ and rate of rotation of 800 r·min-1. Agilent 1701 chromatographic column was used for GC separation and the selected ion monitoring mode was adopted in MS determination. Linearity ranges of the 8 N-nitrosamines were found same between 0.10-2.0 mg·L-1 with the same detection limit (3S/N) of 0.03 mg·kg-1. Tests for recovery and precision were made by standard addition method on the base of blank sample, giving values of recovery and RSD′s (n=6) in the ranges of 73.0%-96.1% and 1.3%-9.7% respectively.

       

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