气相色谱-质谱联用法分析芳纶纤维中残留的N-甲基吡咯烷酮  

Analysis of N-methylpyrrolidinone in aramid fiber by gas chromatography/mass spectrometry method

作　　者：任忠海[1] 李天宝[2] 刘庆备 叶林[2] 

机构地区：[1]广东检验检疫技术中心,广东广州510623 [2]江门出入境检验检疫局,广东江门529000 [3]广东彩艳股份有限公司,广东江门529100

出　　处：《印染助剂》2014年第8期50-52,共3页Textile Auxiliaries

基　　金：广东省科技计划项目(2011B010400019);广东省科技计划项目(2011GDK26)

摘　　要：芳纶纤维在合成过程中常使用N-甲基吡咯烷酮作为反应溶剂,通过对提取方法和色谱、质谱条件的改进,建立了芳纶纤维中溶剂残留物N-甲基吡咯烷酮（NMP）的气相色谱-质谱联用（GC/MS）测定法.芳纶纤维试样经乙酸乙酯超声波提取,提取液浓缩后用滤纸过滤,用气相色谱-质谱仪测定,外标法定量,选择离子监测进行阳性确证.结果表明,当添加N-甲基吡咯烷酮1~10μg/mL时,待测芳纶纤维试样中N-甲基吡咯烷酮的回收率达95.8%,相对标准偏差RSD（n=7）小于5%,其最低检出限为0.05μg/mL.本方法操作简单、灵敏度高、重现性好,可用于芳纶纤维中N-甲基吡咯烷酮残留量分析.N-methylpyrrolidinone （NMP） was commonly used as reaction solvents in the synthesis of ara-mid fiber. A gas chromatography/mass spectrometry （GC/MS） method of determination of N-methylpyrrolidi-none in textiles was established by improving the extraction method and GC/MS conditions. The samples were extracted with ethyl acetate by ultrasound assisted procedure.After being concentrated and purified with filter paper, the extract was quantitatively determined using GC/MS by external standard method and positive-ly confirmed through selected-ion monitoring mode. The results showed that while the dosage of N-methyl-pyrrolidinone was 1~10 μg/mL, the method provided 95.8% of recovery rate, lower than 5% of relative stan-dard deviations and 0.05 μg/mL of determination limit. The method was simple, and had high sensitivity and good repeatability, which could be used in the residual content determination of NMP in aramid fiber.

关 键 词：N-甲基吡咯烷酮 气相色谱-质谱法 芳纶纤维 溶剂残留物 

分 类 号：TQ340.7[化学工程—化纤工业]