Oliveira Hugo M, Segundo Marcela A, Lima José L F C, Cerdà Victor
Faculdade de Farmácia, REQUIMTE, Serviço de Química-Física, Universidade do Porto, Porto, Portugal.
Talanta. 2009 Feb 15;77(4):1466-72. doi: 10.1016/j.talanta.2008.09.036. Epub 2008 Sep 30.
In this work a fast, automatic solid-phase extraction procedure hyphenated to HPLC-UV is proposed for screening of priority phenolic pollutants in waters at ng mL(-1) levels. A flow through column, containing polystyrene-divinylbenzene sorbent, was incorporated to a multisyringe flow injection system (MSFIA), where the sample loading and analyte elution were carried out after computer control. The MSFIA system also directed the eluent to fill the injection loop of the chromatograph, coupling the sample preparation to its determination. High enrichment factors were attained for phenol and ten of its derivatives (mean value 176 for 50 mL of sample), with LOD values lower than 1 ng mL(-1) for the maximum volume of sample used (100mL). For all analytes, mean recoveries between 89 and 103% were obtained for different water matrices. Certified reference material and a contaminated soil (RTC-CRM 112) were also tested successfully. The determination frequency was 4-10h(-1), providing an automatic, fast and reliable tool for water quality and environmental monitoring.
本研究提出了一种与高效液相色谱-紫外联用的快速、自动固相萃取方法,用于筛选水中纳克每毫升(ng mL⁻¹)水平的优先控制酚类污染物。将装有聚苯乙烯-二乙烯基苯吸附剂的流通柱纳入多注射器流动注射系统(MSFIA),在计算机控制下进行样品加载和分析物洗脱。MSFIA系统还引导洗脱液填充色谱仪的进样环,将样品制备与测定过程相结合。苯酚及其十种衍生物获得了较高的富集因子(50 mL样品的平均值为176),对于所用最大样品体积(100 mL),检测限低于1 ng mL⁻¹。对于所有分析物,不同水基质的平均回收率在89%至103%之间。还成功测试了有证标准物质和受污染土壤(RTC-CRM 112)。测定频率为4 - 10次每小时(h⁻¹),为水质和环境监测提供了一种自动、快速且可靠的工具。