涂布纸中邻苯二甲酸酯类增塑剂的快速筛查和半定量分析

Rapid Screening and Semi-quantitative Analyis of Phthalate Plasticizers in Coated Papers

建立了1个快速筛查和半定量分析涂布纸中20种邻苯二甲酸酯类增塑剂含量的气质联用分析方法。本方法采用固体样品直接进样方式,将固体样品置于裂解仪中加热,使涂布纸中的邻苯二甲酸酯类增塑剂释放出来,利用气质联用仪进行在线定性鉴别和半定量分析,外标法定量。对色谱分离条件和裂解器热解吸条件如热解吸温度、热解吸时间、附件初始温度等进行了优化。对方法的检出限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0.03~1.60 mg/kg;相对标准偏差(RSD)为2.71%~14.69%。本方法简单快速,绿色环保,定性准确,灵敏度高,检出限完全满足相关法规的限量要求,可用于涂布纸中邻苯二甲酸酯类增塑剂的快速筛查和半定量分析。

An analytical method was established for the rapid screening and semi-quantitative analysis of 20 kinds of phthalate plasticizers in coated papers using gas chromatography/mass spectrometry(GC/MS) technique. A solid sample direct injection technology was used in the proposed method. The solid sample was placed into the pyrolysis instrument and heated, therefore, phthalate plasticizers in coating papers were released. Then qualitative and semi-quantitative analysis were carried out on-line using GC/MS technique. The external standard method was used to determine the concentration of each phthalate plasticizers. The chromatographic separation conditions were optimized. The working conditions of thermal desorption such as the thermal desorption temperature, the thermal desorption time and the initial temperature of the accessory were also optimized. The limits of detection(LODs) and precision of the proposed method were studied. The limits of detection(LODs) were 10 and 20 mg/kg for DINP and DIDP, respectively. The limits of detection(LODs) changed from 0.03 mg/kg to 1.60 mg/kg for the other 18 phthalate plasticizers. The relative standard deviation(RSDs) changed from 2.71% to 14.69%. The proposed method was simple, fast, environmentally friendly, and reliable and sensitive. The limits of detection(LODs) could meet completely the requirements of relevant regulations. The proposed method could be used in the rapid screening and semi-quantitative analysis of phthalate plasticizers in coated papers.