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首页> 外文期刊>Talanta: The International Journal of Pure and Applied Analytical Chemistry >Microextraction with polyethersulfone for bisphenol-A, alkylphenols and hormones determination in water samples by means of gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry analysis
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Microextraction with polyethersulfone for bisphenol-A, alkylphenols and hormones determination in water samples by means of gas chromatography-mass spectrometry and liquid chromatography-tandem mass spectrometry analysis

机译：气相色谱-质谱和液相色谱-串联质谱法测定聚醚砜微萃取法测定水样中的双酚A，烷基酚和激素

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In the present work, the suitability of polyethersulfone (PES) tube was assessed for the simultaneous sorptive microextraction of commonly found endocrine disrupting compounds in natural waters such as bisphenol-A (BPA), nonylphenol technical mixture (NP mix), 4-tert-octylphenol (4tOP), 4-n-octylphenol (4-nOP), 17 beta-estradiol (E2) and 17 alpha-ethynilestradiol (EE2). After the concentration of target compounds in the PES polymer, the analytes were recovered soaking the polymer with a suitable solvent (ethyl acetate or methanol), derivatized using N,O-bis(trimethylsilyl)trifluoroacetamide with 1% of trimethylchlorosilane (BSTFA+ 1% TMCS) and determined by gas chromatography-mass spectrometry (GC-MS). The analysis was also performed without derivatization step by means of liquid chromatography-tandem mass spectrometry (LC-MS/MS). Extraction parameters (addition of MeOH, ionic strength, extraction speed and time and desorption time) were evaluated and the optimum conditions were fixed as follows: 150 mL water samples containing a 10% (w/v) of sodium chloride and using 5 tubular PES sorbent fibers (1.5 cm length x 0.7 mm o.d.). Equilibrium conditions were achieved after 9 h, with absolute extraction efficiencies ranging from 27 to 56%. On the whole, good apparent recoveries were achieved (68-103% and 81-122% for GC-MS and LC-MS/MS, respectively) using deuterated analogues as surrogates. Achieved quantification limits (LOQs) varied between 2-154 ng/L and 2-63 ng/L for all the compounds using GC-MS and LC-MS/MS, respectively. The effect of organic matter was evaluated previous to apply the final method to the analysis of estuarine and wastewater real samples. The comparison of both methods showed that overall, PES-LC-MS/MS provided shorter sample preparation time and better LODs, but PES-sily/ation-GC-MS allowed the simultaneous determination of all the studied compounds with adequate repeatability and accuracy. (C) 2014 Elsevier B.V. All rights reserved.
机译：在目前的工作中，评估了聚醚砜（PES）管在自然水中常见的内分泌干扰化合物如双酚A（BPA），壬基酚技术混合物（NP mix），4-叔丁基辛基苯酚（4tOP），4-正辛基苯酚（4-nOP），17个β-雌二醇（E2）和17个α-乙炔雌二醇（EE2）。在PES聚合物中浓缩目标化合物后，回收分析物，将聚合物用适当的溶剂（乙酸乙酯或甲醇）浸泡，然后使用N，O-双（三甲基甲硅烷基）三氟乙酰胺与1％的三甲基氯硅烷（BSTFA + 1％TMCS）进行衍生化）并用气相色谱-质谱（GC-MS）测定。还通过液相色谱-串联质谱分析法（LC-MS / MS）在没有衍生化步骤的情况下进行了分析。对萃取参数（MeOH的添加，离子强度，萃取速度，时间和解吸时间）进行了评估，并确定了最佳条件，如下所示：150 mL含10％（w / v）氯化钠的水样品，并使用5个管状PES吸附剂纤维（1.5厘米长x 0.7毫米外径）。 9小时后达到平衡条件，绝对萃取效率为27％至56％。总体而言，使用氘代类似物作为替代物可获得良好的表观回收率（GC-MS和LC-MS / MS分别为68-103％和81-122％）。使用GC-MS和LC-MS / MS分别对所有化合物的定量限（LOQ）在2-154 ng / L和2-63 ng / L之间。事先评估了有机物的影响，以将最终方法应用于河口和废水实际样品的分析。两种方法的比较表明，总体而言，PES-LC-MS / MS提供了更短的样品制备时间和更好的LOD，但PES-sily / ation-GC-MS可以同时测定所有研究的化合物，并具有足够的重复性和准确性。 （C）2014 Elsevier B.V.保留所有权利。

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