GC/MS测定脂肪族二元酸酯类增塑剂干扰消除方法研究  

Study on Interference Elimination Method for Determination of Aliphatic Dicarboxylate Esters Plasticizer by Gas Chromatography/Mass Spectrometry

作　　者：李利荣 吴宇峰 左明 关玉春 LI Lirong;WU Yufeng;ZUO Ming;GUAN Yuchun(Tianjin ECO-Environmental Monitoring Center,Tianjin 300191)

机构地区：[1]天津市生态环境监测中心,天津300191

出　　处：《分析科学学报》2023年第6期705-710,共6页Journal of Analytical Science

基　　金：国家环境保护标准制修订项目(2021-12)资助。

摘　　要：本文优化了气相色谱/质谱法(GC/MS)测定高背景干扰试样中11种脂肪族二元酸酯类(ADEs)增塑剂的干扰消除方法。以污水中11种ADEs的净化方法为例,通过洗脱实验和加标回收率,对比了不同配比二氯甲烷/正己烷、丙酮/正己烷和乙酸乙酯/正己烷3种洗脱溶剂体系对不同品牌弗罗里硅土、硅胶和氧化铝固相萃取柱(SPE)的洗脱特性,并探讨了分离、检测过程中常见其他半挥发有机物对GC/MS的影响。结果发现3种类型SPE均可作为ADEs的净化柱,乙酸乙酯/正己烷体系的洗脱效率明显高于二氯甲烷/正己烷和丙酮/正己烷,相同溶剂对不同品牌的同一类型净化柱洗脱回收率可能存在较大的差异,使用前需通过淋洗曲线确定最佳的洗脱溶剂组成。16种邻苯二甲酸酯(PAEs)、64种半挥发性有机物(SVOCs)和31种石油烃(TPH)均不对11种ADEs的GC/MS定性定量造成干扰。在优化的净化条件下,11种ADEs的回收率为80.2%~115%,相对标准偏差为5.2%~15%。本方法简单、快速,具有较好的重现性和回收率,可用于污水等高污染样品中ADEs的检测分析。The cleanup method for the determination of 11 aliphatic dicarboxylate esters(ADEs)plasticizer in samples with high matrix interference by gas chromatography/mass spectrometry(GC/MS)was optimized.Taking 11 ADEs in sewage cleanup method as an example,the cleanup characteristics of different brands of Florisil,silica gel and alumina solid phase extraction(SPE)cartridges by dichloromethane/n-hexane,acetone/n-hexane and ethyl acetate/n-hexane elution solution were compared respectively through elution experiments and spiked ADEs recovery.The influences of other common semivolatile organic compounds(SVOCs)in separation and detection process by GC/MS were discussed.The results showed that the three types of SPE cartridges can all be used for the cleanup of ADEs according to the disturbance characteristics.The elution efficiency of ethyl acetate/n-hexane system was significantly more efficient than that of dichloromethane/n-hexane and acetone/n-hexane.Different brands of the same type of SPE cartridges might have distinct differences elution results.Before use,the best elution solvent composition should be determined through the elution curve inspection.Sixteen phthalates(PAEs),64 SVOCs and 31 petroleum hydrocarbons(TPHs)did not interfere with the qualitative and quantitative analysis of 11 ADEs by GC/MS.Under the optimized conditions,the spiked recoveries of 11 ADEs were between 80.2%-115%,and the relative standard deviations were between 5.2%-15%.This method is simple,rapid and efficient with good reproducibility,and can be used for the detection of ADEs in high interference matrix such as sewage.

关 键 词：脂肪族二元酸酯类化合物 污水 高背景干扰 固相萃取柱净化 气相色谱/质谱法 

分 类 号：O657.63[理学—分析化学]