固相萃取-气相色谱法检测纺织品中的邻苯二甲酸酯

摘要

In view of the problem of difficult enrichment and high detection limit of phthalate esters (PAEs),the method of solid phase extraction (SPE)and gas chromatography (GC)was established for the determination of phthalate esters in textiles.Through comparison of four kinds of solid phase extractant eluting agent type,eluent amount,sample and the elution rate, the optimal extraction conditions were determined as:C18 column as extraction agent,3mL methanol and 3 mL ultrapure water are sequentially activated,the sample rate of 1 mL/min,e-lution solvent is hexane acetone (30∶1,V/V),the elution solvent dosage is 3mL,elution rate 1 mL/min.The method has a good relationship in the low concentration range.The recoveries of spiked samples range from 84% to 102%,and the relative standard deviation (RSD)is less than 5%.DMP,DEP and DBP minimum detection limit respectively is 0.014mg/L,0.015mg/L and 0.018mg/L.The method can quickly and effectively detect the PAEs of actual textile samples.%针对邻苯二甲酸酯(PAEs,phthatate esters)富集效率低和检测限高的问题,建立固相萃取(SPE,solid-phase extraction)-气相色谱(GC,gas chromatography)联用法检测纺织品中邻苯二甲酸酯的方法.通过比较4种固相萃取剂的洗脱剂种类、洗脱剂用量、上样和洗脱速率,最后确定最优萃取条件为：C18柱为萃取剂,3mL 甲醇和3mL 重蒸馏水依次活化,上样速率1mL/min,洗脱溶剂为正己烷-丙酮(30∶1,V/V),洗脱溶剂3mL,洗脱速率为1mL/min.该方法在低浓度范围内线性关系良好,加标回收率为84%~102%,相对标准偏差小于5%,DMP、DEP 和 DBP 的最低检出限分别是0.014mg/L、0.015mg/L和0.018mg/L,能快速有效地检测实际纺织样品的邻苯二甲酸酯类物质.