气相色谱-质谱联用内标法测定土壤中11种酞酸酯  

Determination of phthalic acid esters in soil samples by gas chromatography-mass spectrometry with internal standard method

作　　者：黄玉娟[1] 陈永山[1] 骆永明[1,2] 章海波[1] 宋静[1] 

机构地区：[1]中国科学院土壤环境与污染修复重点实验室,南京土壤研究所,南京210008 [2]中国科学院烟台海岸带研究所,烟台264003

出　　处：《环境化学》2013年第4期658-665,共8页Environmental Chemistry

基　　金：国家水体污染控制与治理科技重大专项课题(2008ZX07101-006-05);中国科学院“优秀博士学位论文;院长奖获得者科研启动专项资金”资助

摘　　要：建立了土壤中11种酞酸酯(PAEs)的气相色谱-质谱联用(GC-MS)内标分析方法,通过优化色谱柱升温程序和载气流量后,11种酞酸酯在18 min内得到良好的分离.同时以连续7次进样后计算PAEs峰面积响应值和峰面积变异系数为衡量指标,并逐个优化GC-MS的进样口温度、GC与MS的接口温度、进样方式和进样体积等GC-MS仪器操作参数,确定了GC-MS分析PAEs的最优条件为进样口温度250℃,接口温度280℃,载气流速1.2 mL.min-1,进样体积1.0μL,非脉冲进样方式.该分析条件下PAEs各组分的检出限(S/N=3)为0.37—1.97μg.L-1.该分析方法用于土壤样品中酞酸酯含量分析,并用苯甲酸苄酯(BenzylBenzoate)作为内标物,用内标法对11种肽酸酯进行定量,方法检出限0.01—0.07 mg.kg-1,土壤加标回收率基本在93.0%—115.0%范围内,结果可行.This work was conducted to develop a method for the determination of 11 phthalic acid esters （PAEs） by gas chromatography-mass spectrometry with internal standard substance, and the separation of the 11 PAEs was achieved by optimization of the oven temperature program and the carrier gas flow rate. After seven repeated sample injections, the response values （R） and coefficient of variation （CV） of PAE peak area were calculated, by changing some of the instrument parameters such as inlet temperature, the interface temperature between GC and MS, injection methods, and the volume injected. The optimal conditions, of the GC-MS for analysis of PAEs were as follows ： the inlet temperature was 250℃, the interface temperature between GC and MS was 280 ℃, the carrier gas flow rate was 1.2 mL· min^-1, the volume injection was 1.0 μL and the injection method was non-pulsed. Under the optimal conditions, the detection limit of 11 PAEs was from 0.37 to 1.97 μg· L-1. This method was then used for analysis of PAEs in soil samples using Benzyl benzoate as internal standard for quality assurance and high sensitivity. The detection limits of the PAEs in soil samples were 0.01---0. 07 mg.kg-1 and the spiked recoveries were in the range of 93.0%--115.0%.

关 键 词：气相色谱-质谱联用 酞酸酯 土壤 

分 类 号：X833[环境科学与工程—环境工程] O657.63[理学—分析化学]