气相色谱-质谱法测定橡胶产品中两种N-亚硝胺

Determination of two N-nitrosamines in rubber materials by gas chromatography-mass spectrometry

建立了橡胶材料中N-亚硝基甲基苯胺和N-亚硝基乙基苯胺的气相色谱-质谱检测方法。探讨了检测过程中产生N-亚硝基甲基苯胺和N-亚硝基乙基苯胺假阳性的原因,研究了进样口温度对检测结果的影响。实验数据表明,进样口温度较高时,N-亚硝基甲基苯胺和N-亚硝基乙基苯胺会在进样口处分解为N-甲基苯胺和N-乙基苯胺。进样口温度设置为150℃时,N-亚硝基甲基苯胺和N-亚硝基乙基苯胺在进样口处仅轻度分解,且此时两种物质质量浓度在0. 5~10 mg/L范围内线性关系良好,线性相关系数分别为0. 9992和0. 9997,加标回收率为100%~115%,RSD小于10%。阳性样品和假阳性样品测试结果表明,此方法可有效提高定性结果的准确性,避免假阳性的结果,满足检测需求。

In this study,a gas chromatography-mass spectrometry method was developed for the determination of N-nitroso-N-methyl-N-phenylamine and N-nitroso-N-ethyl-N-phenylamine in rubber materials.The reason for the false positive result produced during the detection process was investigated.In addition,the influence of the inlet temperature of GC on the test results was studied.The results showed that when the inlet temperature was high,N-nitroso-N-methyl/ethyl-N-phenylamine would be decomposed into N-methylaniline and N-ethylaniline.When the inlet temperature was set to150℃,the decomposition of N-nitroso-N-methyl-N-phenylamine and N-nitroso-N-ethyl-N-phenylamine was in the low level,meanwhile a satisfied linearity was remained in the range of 0.5-10 mg/L with the correlation coefficiency(R2)of 0.9992 and 0.9997,respectfully.The test results of positive samples and false positive samples indicated that this method can effectively improve the determination accuracy,avoid the false positive results and meet the detection requirements.