Escola de Química e Alimentos, Universidade Federal do Rio Grande, Rio Grande, RS, Brazil.
J Sep Sci. 2013 Oct;36(20):3411-8. doi: 10.1002/jssc.201300599. Epub 2013 Sep 1.
This work reports the development of a dispersive liquid-liquid microextraction method for the simultaneous extraction, preconcentration, and derivatization of Hg(2+) and CH3Hg(+) species from water samples for further determination by GC-MS. Some parameters of the proposed method, such as volume and type of disperser and extraction solvent, and Na[B(C6H5)4] concentration were investigated using response surface methodology. Suitable recoveries were obtained using 80 μL C2 Cl4 (as extraction solvent), 1000 μL ethanol (as disperser solvent), and 300 μL 2.1 mmol/L Na[B(C6H5)4] (as derivatizing agent). Accuracy was evaluated in terms of recovery and ranged from 87 to 99% with RSD values <7%. In addition, a certified reference material of water (NIST 1641d) was analyzed and agreed with the certified value about 107% (for Hg(2+)), with RSD values <8.5%. LODs were 0.3 and 0.2 μg/L, with enrichment factors of 112 and 115 for Hg(2+) and CH3Hg(+), respectively. The optimized method was applied for the determination of Hg(2+) and CH3Hg(+) in tap, well, and lake water samples.
本工作报道了一种分散液液微萃取方法的发展,用于从水样中同时萃取、预浓缩和衍生 Hg(2+)和 CH3Hg(+),以便进一步用 GC-MS 测定。使用响应面法研究了该方法的一些参数,如分散剂和萃取溶剂的体积和类型,以及 Na[B(C6H5)4]浓度。使用 80 μL C2 Cl4(作为萃取溶剂)、1000 μL 乙醇(作为分散剂溶剂)和 300 μL 2.1 mmol/L Na[B(C6H5)4](作为衍生化剂),可以获得合适的回收率。准确度通过回收率进行评估,范围为 87%至 99%,RSD 值<7%。此外,还分析了一种水的认证参考物质(NIST 1641d),并与认证值约 107%(对于 Hg(2+))一致,RSD 值<8.5%。LOD 分别为 0.3 和 0.2 μg/L,Hg(2+)和 CH3Hg(+)的富集因子分别为 112 和 115。优化后的方法用于测定自来水中的 Hg(2+)和 CH3Hg(+)、井水和湖水样本。