热解吸-气质联用法快速筛查涂层织物中的邻苯二甲酸酯类增塑剂

Rapid screening of phthalate plasticizers in coated fabrics by thermal desorption-gas chromatography/mass spectrometry

采用固体样品直接进样技术,利用裂解仪的热解吸功能,通过加热将待测样品中的目标分析物释放出来,并在线利用气质联用仪进行定性、半定量分析,外标法定量,从而建立了1个快速鉴别和测定涂层织物中20种邻苯二甲酸酯类增塑剂残留量的气质联用分析方法,并对热解吸温度、热解吸时间、附件初始温度等裂解器热解吸工作条件和仪器分析条件进行了优化,对方法的线性关系和精密度进行了研究。DINP和DIDP的检出限分别为10、20mg/kg,其余18种邻苯二甲酸酯类增塑剂的检出限为0.03~1.60mg/kg。方法的精密度实验相对标准偏差为2.47~14.31%。该方法不需使用任何有机溶剂进行前处理,绿色环保,对环境友好。该方法简单快速、定性可靠、灵敏度高,检出限完全满足相关法规的限量要求,可用于涂层织物中邻苯二甲酸酯类增塑剂的定性初筛。

The target analyte in the sample to be tested was first released by heating based on the thermal desorption function of the pyrolysis instrument,using solid sample direct injection technology,then qualitative and semi-quantitative analysis were performed on-line using gas chromatography/mass spectrometry(GC/MS)technique.The concentration of each phthalate plasticizers were calibrated by the external standard method.Therefore,a GC/MS method for the rapid identification and determination of 20 phthalate plasticizer residues in coated fabrics was established.The instrumental analysis conditions and the working conditions of thermal desorption such as thermal desorption temperature,thermal desorption time,initial temperature of the accessory were optimized.The linear relationship and precision of the method were studied.The limits of detection(LODs)of DINP and DIDP were 10 and 20mg/kg,respectively and the limits of detection(LODs)of the other 18 phthalate plasticizers varied from 0.03mg/kg to 1.60 mg/kg.The relative standard deviation of the precision experiments changed from 2.47%to 14.31%.The method did not need any organic solvent for pretreatment and was environmentally friendly.The method was simple,rapid,sensitive and reliable.The limits of detection(LODs)met completely the requirements of relevant regulations,and could be used for the qualitative screening of phthalate plasticizers in coated fabrics.