Department of Environmental Engineering, Gebze Institute of Technology, Kocaeli, Turkey.
J Sep Sci. 2012 Dec;35(24):3561-8. doi: 10.1002/jssc.201200550.
This article introduces a simple, rapid, and reliable solid-phase microextraction (SPME) method coupled with GC-MS for the quantitative determination of 16 polycyclic aromatic hydrocarbons in water. In this study, the Taguchi experimental design was used to optimize extraction conditions of polycyclic aromatic hydrocarbons using SPME method to obtain highly enriched analytes. Consequently, quantitative determination of polycyclic aromatic hydrocarbons in water was achieved by GC-MS technique. The selected parameters affecting enrichment of polycyclic aromatic hydrocarbons were sample extraction time, stirring speed, temperature, ionic strength, and pH. The study revealed that optimal operating conditions were found to be 90-min extraction time, 1400 rpm stirring speed, and 60°C sample temperature. The effect of ionic strength and pH were shown to be insignificant. Optimized conditions were also reevaluated by placing the 16 polycyclic aromatic hydrocarbons into several subgroups based on their molecular weight. The extraction efficiency of polycyclic aromatic hydrocarbons with low molecular weight was shown to be a function of only the extracting temperature. Satisfactory results were obtained for linearity (0.983-0.999), detection limits (2.67-18.02 ng/L), accuracy (71.2-99.3%), and precision (4.3-13.5%). The optimum conditions reported by other design approaches were evaluated and generalized optimum conditions were suggested.
本文介绍了一种简单、快速、可靠的固相微萃取（SPME）方法，并结合 GC-MS 定量测定水中的 16 种多环芳烃。本研究采用田口实验设计优化了 SPME 法萃取水中多环芳烃的条件，以获得高度富集的分析物。然后，通过 GC-MS 技术实现了水中多环芳烃的定量测定。选择了影响多环芳烃富集的参数，包括样品萃取时间、搅拌速度、温度、离子强度和 pH 值。研究表明，最优的操作条件为萃取时间 90 min、搅拌速度 1400 rpm 和样品温度 60°C。离子强度和 pH 值的影响可以忽略不计。通过将 16 种多环芳烃根据分子量分为几个亚组，对优化条件进行了重新评估。低分子量多环芳烃的萃取效率仅与萃取温度有关。线性范围（0.983-0.999）、检测限（2.67-18.02 ng/L）、准确度（71.2-99.3%）和精密度（4.3-13.5%）均令人满意。还评估了其他设计方法报告的最佳条件，并提出了通用的最佳条件。
