Wang Yonghua, Li Yongqiang, Feng Jianfang, Sun Cheng
State Key Laboratory of Pollution Control and Resource Reuse, School of the Environment, Nanjing University, Nanjing 210093, China.
Anal Chim Acta. 2008 Jul 7;619(2):202-8. doi: 10.1016/j.aca.2008.05.003. Epub 2008 May 8.
A headspace solid-phase microextraction (HS-SPME) coupled with gas chromatography and flame ionization detector (GC-FID) was applied to determine seven benzene derivatives in water samples. A polyaniline (PANI) fiber which was electrochemically coated on a stainless steel wire was employed to extract the target analytes from aqueous system. Five experimental parameters consisting of adsorption temperature, adsorption time, stirring rate, salt concentration and headspace volume were evaluated and optimized by means of a Taguchi's L(16) (4(5)) orthogonal array experimental design. The experimental results indicated that adsorption temperature and salt concentration were the most significant factors in the analysis procedure. The optimized conditions were as follows: 20 degrees C of adsorption temperature, a constant stirring speed of 600 rpm and 20 min of extraction carried out in 10 mL of water samples saturated with NaCl. The proposed method was linear approximately three orders (0.1-100 microgL(-1)) of magnitude for the tested compounds, with linear correlation coefficients (r(2)) greater than 0.98. Relative standard deviation ranged from 5.3 to 8.4% and limit of detection was relatively low (0.01-0.06 microgL(-1)). The proposed method was applied to determine the trace level compounds in natural water samples.
采用顶空固相微萃取（HS-SPME）结合气相色谱和火焰离子化检测器（GC-FID）测定水样中的七种苯衍生物。使用电化学涂覆在不锈钢丝上的聚苯胺（PANI）纤维从水体系中萃取目标分析物。通过田口的L(16) (4(5)) 正交阵列实验设计评估并优化了吸附温度、吸附时间、搅拌速率、盐浓度和顶空体积这五个实验参数。实验结果表明，吸附温度和盐浓度是分析过程中最显著的因素。优化条件如下：吸附温度为20℃，恒定搅拌速度为600 rpm，在10 mL用NaCl饱和的水样中进行20分钟萃取。所提出的方法对被测化合物的线性范围约为三个数量级（0.1 - 100 μg L(-1)），线性相关系数（r(2)）大于0.98。相对标准偏差范围为5.3%至8.4%，检测限相对较低（0.01 - 0.06 μg L(-1)）。所提出的方法用于测定天然水样中的痕量化合物。
