Naccarato Attilio, Gionfriddo Emanuela, Sindona Giovanni, Tagarelli Antonio
Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via P. Bucci Cubo 12/C, I-87030 Arcavacata di Rende (CS), Italy.
Dipartimento di Chimica e Tecnologie Chimiche, Università della Calabria, Via P. Bucci Cubo 12/C, I-87030 Arcavacata di Rende (CS), Italy.
J Chromatogr A. 2014 Apr 18;1338:164-73. doi: 10.1016/j.chroma.2014.02.089. Epub 2014 Mar 12.
This work proposes a new approach for the simultaneous determination of benzothiazoles, benzotriazoles and benzosulfonamides in different environmental matrices and human urine, using solid-phase microextraction coupled with gas-chromatography-triple quadrupole mass spectrometry (SPME-GC-QqQMS). The analytes object of this investigation have been classified as toxic to aquatic organisms and their presence in human urine was reported to occur as result of human exposure to contaminated environment. In this work many of the challenges related to the chemical diversity and polarity of the analytes selected were overcame conducting a multivariate optimization of the working conditions by using the approach of "Experimental design". Tests performed to assess the performances of five SPME coatings in direct immersion mode revealed the polyacrylate coating to be the most suitable for the extraction of the probe analytes. A central composite design (CCD) was employed to determine the optimal conditions for four factors affecting the solid-phase microextraction process: extraction time, extraction temperature, pH and percentage of sodium chloride. The optimal working condition determined by using Derringer's desirability function were 40min as extraction time, pH 7.1 and 6.0% of NaCl. Since the extraction temperature do not significantly affects the responses for all the analytes considered, analyses were performed at room temperature. A careful evaluation of the matrix effect for all the matrices tested was carried out. The results obtained showed that the proposed method did not significantly influenced by matrix effects in most of the cases tested, and thus allows the use of simplified calibration procedure. Satisfactory values of accuracy and precision were also obtained for all the matrices considered.
本研究提出了一种新方法，采用固相微萃取结合气相色谱-三重四极杆质谱联用技术（SPME-GC-QqQMS），同时测定不同环境基质和人体尿液中的苯并噻唑、苯并三唑和苯磺酰胺。本研究的分析物被归类为对水生生物有毒，据报道，人体尿液中这些物质的存在是由于人类接触受污染环境所致。在这项工作中，通过“实验设计”方法对工作条件进行多变量优化，克服了与所选分析物的化学多样性和极性相关的许多挑战。对五种直接浸入式SPME涂层性能进行的测试表明，聚丙烯酸酯涂层最适合萃取目标分析物。采用中心复合设计（CCD）来确定影响固相微萃取过程的四个因素的最佳条件：萃取时间、萃取温度、pH值和氯化钠百分比。使用Derringer合意函数确定的最佳工作条件为：萃取时间40分钟、pH值7.1和氯化钠含量6.0%。由于萃取温度对所有考虑的分析物的响应影响不显著，因此在室温下进行分析。对所有测试基质的基质效应进行了仔细评估。所得结果表明，在大多数测试案例中，所提出的方法受基质效应的影响不显著，因此可以使用简化的校准程序。对于所有考虑的基质，还获得了令人满意的准确度和精密度值。
