气相色谱-质谱联用法测定童鞋中N-甲基吡咯烷酮和N-乙基吡咯烷酮  

Determination of N-methyl-2-pyrrolidone and N-ethyl-2-pyrrolidone in children's footwear by gas chromatography-mass spectrometry

作　　者：郝晓红 马红青[1] 肖湾 HAO Xiaohong;MA Hongqing;XIAO Wan(Institute of Quality Inspection of Light Industry&Chemical products,Shanghai Institute of quality Inspection and Technical Research,Shanghai 201114,China)

机构地区：[1]上海市质量监督检验技术研究院,轻工与化工产品质量检验所,上海201114

出　　处：《化学分析计量》2024年第10期39-44,共6页Chemical Analysis And Meterage

基　　金：上海市科学技术委员会研发公共服务平台建设项目(14DZ2293000)。

摘　　要：建立了气相色谱-质谱联用(GC-MS)法同时测定童鞋中N-甲基吡咯烷酮和N-乙基吡咯烷酮。童鞋产品中常用的材料有纺织品、合成革、皮革和乙烯-乙酸乙烯酯共聚物材料。取童鞋中不同材质的样品,优化了预处理过程,确定预处理条件为50℃用丙酮超声提取60 min,根据不同材质提取液情况选择是否需要净化。取适量提取液供GC-MS仪分析,以色谱峰面积为纵坐标,质量浓度为横坐标,外标法定量。该方法检出限为0.5 mg/kg,N-甲基吡咯烷酮和N-乙基吡咯烷酮的质量浓度在0.5~50 mg/L范围内与色谱峰面积具有良好的线性关系,线性相关系数均大于0.9995,低、中、高三个浓度水平的加标回收率为96.3%~98.7%,测定结果的相对标准偏差为0.2%~1.8%(n=7),满足测定要求。A method for determination of N-methylpyrrolidone(NMP)and N-ethylpyrrolidone(NEP)in children's shoes by gas chromatography and mass spectrometry(GC-MS)was established.The commonly used materials in children's shoes are textiles,synthetic leather,leather and EVA materials.Samples of different materials in children's shoes were taken to optimize the pretreatment process,including the solvent,ultrasonic extraction time and temperature.Finally,the ultrasonic extraction was carried out in 50℃water bath for 60 min with acetone.and whether purification was required according to the extraction liquid of different materials.Appropriate amount of extraction liquid was obtained for GC-MS analysis.The peak area was taken as the vertical coordinate and the concentration was taken as the horizontal coordinate.The detection limit of the method was 0.5 mg/kg.It is showed that there is a good linear relationship in the range of 0.5-50 mg/L of N-methylpyrrolidone and N-ethylpyrrolidone,the linear correlation coefficients were all greater than 0.9995.The recoveries of low,medium and high concentrations were 96.3%-98.7%.The relative standard deviation of the measured results was 0.2%-1.8%(n=7),which met the determination requirements.

关 键 词：气相色谱-质谱联用 童鞋 N-甲基吡咯烷酮 N-乙基吡咯烷酮 

分 类 号：O657[理学—分析化学]