Pressurized liquid extraction of organophosphate triesters from sediment samples using aqueous solutions
Pressurized liquid extraction of organophosphate triesters from sediment samples using aqueous solutions
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DOI：
10.1016/j.chroma.2009.08.068
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发表时间：
2009-10-16
影响因子：
4.1
通讯作者：
Cela, R.
中科院分区：
文献类型：
--
作者：
Garcia-Lopez, M.;Rodriguez, I.;Cela, R.
开发了一种从沉积物样品中提取用作阻燃剂和增塑剂的七种有机磷酸三酯（OP）的新方法。它是基于加压液体萃取的分析物与水溶液，结合进一步的浓缩步骤，使用固相萃取（SPE），然后通过气相色谱-质谱联用（GC-MS）测定。系统地评价了不同变量对样品制备过程的产率和选择性的影响。观察到的最佳响应是在90 ℃和1500 psi下用水：乙腈（75：25）溶液提取2 g沉淀物5 min。用超纯水将所得提取物补足至200 mL，并通过OASIS HLB，60 mg柱。用2 mL乙酸乙酯回收分析物，并将该萃取物浓缩至较低体积，约100 mL。0.2 mL.该方法的回收率为77%~ 111%，相对标准偏差小于10%，适用于总碳含量（TC）高达4.0%的河流和海洋沉积物样品。该方法的定量限（LOQ）在0.5和5 ng g（-1）之间变化。对未加标的沉积物样品进行的分析表明，一些被调查物种的浓度水平较低，最高浓度（47纳克/克）对应于磷酸三（2-氯乙基）酯（TCEP）。(C)2009爱思唯尔有限公司版权所有。
A novel procedure for the extraction of seven organophosphate triesters (OPs), used as flame retardants and plasticizers, from sediment samples has been developed. It is based on the pressurized liquid extraction of the analytes with aqueous solutions, combined with a further concentration step using solid-phase extraction (SPE) and followed by gas chromatography coupled to mass spectrometry (GC-MS) determination. The effects of different variables on the yield and selectivity of the sample preparation process are systematically evaluated. The optimal responses were observed extracting 2g of sediment with a water:acetonitrile (75:25) solution at 90 degrees C and 1500 psi for 5 min. The obtained extract was made up to 200 mL with ultrapure water and passed through an OASIS HLB, 60 mg cartridge. Analytes were recovered with 2 mL of ethyl acetate and this extract concentrated to a lower volume, ca. 0.2 mL. Recoveries of the proposed extraction method ranged from 77 to 111%, with relative standard deviations below 10%, for spiked river and marine sediment samples with total carbon contents (TC) up to 4.0%. The limits of quantification (LOQs) of the method varied between 0.5 and 5 ng g(-1). Analysis of non-spiked sediment samples revealed the presence of low levels for some of the investigated species, with the highest concentration (47 ng g(-1)) corresponding to tris(2-chloroethyl) phosphate (TCEP). (C) 2009 Elsevier B.V. All rights reserved.