Abstract:
Phthalic acid esters (PAEs) are emerging pollutants that need to be analyzed precisely. Chromatography-based determination of PAE content in soils are frequently affected by matrix effect, which may limit the quantification of different kinds of PAEs from different types of soil. Here we optimized a QuEChERS protocol combined with gas chromatography-mass spectrometry (GC-MS) for simultaneous determination of 16 PAEs in different soils. PAEs in different type of soils (fluvo-aquic soil, red soil, and black soil) were extracted with acetonitrile followed by GC-MS detection based on quantitative ion internal standard method. All 16 PAEs showed excellent linear relationships with mass peak areas (R2 > 0.99). The limits of detection (LOD) and limits of quantitation (LOQ) of all the samples were in the range of 0.91-66.97 µg/kg and 2.7-200.9 µg/kg, respectively. The accurate test at 0.5, 0.1, and 1.0 mg/kg spiking level recorded recovery rate between 80.11% and 100.99% with relative standard deviations (RSDs) ranging from 0.37 to 8.50% in tested matrices. No significant matrix effect was observed for most tested PAEs. This is a simple method with high sensitivity and strong stability, which is suitable and reproducible for quantifying large number of PAEs in different types of soil.
摘要:
邻苯二甲酸酯(PAEs)是需要精确分析的新兴污染物。基于色谱法的土壤中PAE含量测定经常受到基体效应的影响,这可能会限制不同类型土壤中不同类型PAEs的定量。在这里,我们优化了QuEChERS协议与气相色谱-质谱联用(GC-MS),用于同时测定不同土壤中的16种PAEs。不同类型土壤中的PAEs(潮土,红壤,和黑土)用乙腈提取,然后基于定量离子内标法进行GC-MS检测。所有16种PAEs均与质量峰面积呈良好的线性关系(R2>0.99)。所有样品的检测限(LOD)和定量限(LOQ)均在0.91-66.97µg/kg和2.7-200.9µg/kg范围内,分别。在0.5、0.1和1.0mg/kg加标水平下的准确测试记录的回收率在80.11%至100.99%之间,测试基质中的相对标准偏差(RSD)为0.37%至8.50%。对于大多数测试的PAEs没有观察到显著的基质效应。这是一种简单的方法,灵敏度高,稳定性强,适用于定量不同类型土壤中的大量PAEs。