气相色谱-质谱法测定电线电缆中苯二甲酸酯类增塑剂  

Determination of Phthalate Plasticizers in Wires and Cables by Gas Chromatography-mass Spectrometry

作　　者：蒋武 张达 翁振杰 卢立用 Jiang Wu;Zhang Da;Weng Zhenjie;Lu Liyong(Wenzhou Technical Testing Research Institute for Quality,Wenzhou,Zhejiang 325000,China)

机构地区：[1]温州市质量技术检测科学研究院,浙江温州325000

出　　处：《塑料助剂》2024年第2期14-19,31,共7页Plastics Additives

基　　金：温州市质检院院级科研项目(2021009)。

摘　　要：在电线电缆中大量应用的苯二甲酸酯类增塑剂可能造成人体内分泌失调,但目前研究主要集中于邻苯二甲酸酯类的检测。随着法规趋严,替代品的应用随之增加,为此建立了测定电线电缆中14种邻、间、对苯二甲酸酯增塑剂含量的气相色谱-质谱检测法。将电线电缆外皮冷冻粉碎至粒径小于1 mm,以10 mL乙酸乙酯为提取溶剂,60℃下超声萃取40 min,提取液用0.45μm有机相滤膜过滤后,选择离子监测(SIM)模式下,以特征碎片离子丰度比定性,内标法定量。结果显示,14种苯二甲酸酯增塑剂在0.20~20.0 mg/L浓度范围内具有较好的线性,相关系数均大于0.995,检出限为0.2~1.0 mg/kg,对空白样品进行加标回收实验,回收率为93.1%~120.2%,相对标准偏差为0.8%~7.6%。本方法用10个样品分析,均检出苯二甲酸酯增塑剂。Phthalate plasticizers are widely used in wires and cables,which may cause endocrine disorders in the human body.However,current research mainly focuses on the detection of phthalatic esters(PAEs).As regulations are becoming stricter,the application of substitutes is increasing.Therefore,a gas chromatography-mass spectrometry detection method was established to determine the contents of 14 types of phthalate plasticizers in wires and cables.The outer plastics of wires and cables were frozen and crushed until the particle size was less than 1 mm.Use 10 mL of ethyl acetate as the extraction solvent and perform ultrasonic extraction at 60 C for 40 minutes.After the extract was filtered with the membrane with the diameter of 0.45μm,selective ion monitoring(SIM)mode was adopted to determine the target compounds.Qualitative analysis using characteristic fragment ion abundance ratio and quantitative analysis using internal standard method.The results were achieved as follows.14 types of phthalate plasticizers had good linearity in the range of 0.20-20.0 mg/L,and their correlation coefficients were all greater than 0.995 with the detection limits within the range of 0.2-1.0 mg/kg.Spiked recovery tests were performed on blank samples,with a recovery rate of 93.1%-120.2% and a relative standard deviation of 0.8%-7.6%.In conclusion,when applying this method to experiments,we detected phthalate plasticizers in all10 samples.

关 键 词：气相色谱-质谱法 苯二甲酸酯 增塑剂 电线电缆 

分 类 号：O657.63[理学—分析化学] TM246[理学—化学]