Department of Chemistry, National Central University, Chung-Li 320, Taiwan.
Talanta. 2011 Apr 15;84(2):406-10. doi: 10.1016/j.talanta.2011.01.055. Epub 2011 Jan 26.
The rapid and solvent-free determination of organophosphate esters (OPEs) in aqueous samples via one-step microwave-assisted headspace solid-phase microextraction (MA-HS-SPME) followed by gas chromatography-mass spectrometry (GC-MS) analysis is described. Tri-n-butyl phosphate (TnBP) and tris-(2-ethylhexyl) phosphate (TEHP) were selected as model compounds for the method of development and validation. The effects of various extraction parameters for the quantitative extraction of these analytes by MA-HS-SPME were systematically investigated and optimized. The analytes, in a 20 mL water sample (in a 40 mL sample bottle containing 2g of NaCl, pH 3.0), were efficiently extracted by a polydimethylsiloxane-divinylbenzene (PDMS-DVB) fiber placed in the headspace when the system was microwave irradiated at 140 W for 5 min. The limits of quantification (LOQs) for TnBP and TEHP were 0.5 and 4 ng/L, respectively. Using the standard addition method, MA-HS-SPME coupled with GC-MS was utilized to determine selected OPEs in surface water and wastewater treatment plants (WWTP) influent/effluent samples. Preliminary results show that TnBP was commonly detected OPEs in these aqueous samples, the correlation coefficients (r(2)) of the standard addition curves were greater than 0.9822, indicating that the developed method appears to be a good alternative technique for analyzing OPEs in aqueous samples.
描述了一种通过一步微波辅助顶空固相微萃取（MA-HS-SPME），然后进行气相色谱-质谱（GC-MS）分析，快速、无溶剂测定水样中有机磷酸酯（OPEs）的方法。三正丁基磷酸酯（TnBP）和三（2-乙基己基）磷酸酯（TEHP）被选为方法开发和验证的模型化合物。系统研究和优化了各种萃取参数对这些分析物通过 MA-HS-SPME 进行定量萃取的影响。在微波辐射 140 W 5 分钟的条件下，将 20 mL 水样（在含有 2 g NaCl 的 40 mL 样品瓶中，pH 值为 3.0）置于顶空，用 PDMS-DVB 纤维有效地萃取这些分析物。TnBP 和 TEHP 的检出限（LOQs）分别为 0.5 和 4 ng/L。使用标准添加法，MA-HS-SPME 与 GC-MS 联用，用于测定地表水中和污水处理厂（WWTP）进水/出水样品中的选定 OPEs。初步结果表明，TnBP 是这些水样中常见的 OPEs，标准添加曲线的相关系数（r(2)）大于 0.9822，表明该方法似乎是一种分析水样中 OPEs 的良好替代技术。
