Wang Xiaowei, Luo Lijuan, Ouyang Gangfeng, Lin Li, Tam Nora F Y, Lan Chongyu, Luan Tiangang
State Key Laboratory of Biocontrol/MOE Key Laboratory of Aquatic Product Safety, School of Life Sciences, Sun Yat-Sen University, Guangzhou 510275, China.
J Chromatogr A. 2009 Aug 28;1216(35):6267-73. doi: 10.1016/j.chroma.2009.07.011. Epub 2009 Jul 15.
A sample pretreatment method for the determination of 18 chlorophenols (CPs) in aqueous samples by derivatization liquid-phase microextraction (LPME) was investigated using gas chromatography-mass spectrometry. Derivatization reagent was spiked into the extraction solvent to combine derivatization and extraction into one step. High sensitivity of 18 CPs derivatives could be achieved after optimization of several parameters such as extraction solvent, percentage of derivatization reagent, extraction time, pH, and ionic strength. The results from the optimal method showed that calibration ranging from 0.5 to 500microgL(-1) could be achieved with the RSDs between 1.75% and 9.39%, and the limits of detection (LOD) are ranging from 0.01 to 0.12microgL(-1) for the CPs. Moreover, the proposed LPME method was compared with solid-phase microextraction (SPME) coupled with on-fiber derivatization technique. The results suggested that using both methods are quite agreeable. Furthermore, the recoveries of LPME evaluated by spiked environmental samples ranged from 87.9% (3,5-DCP) to 114.7% (2,3,5,6-TeCP), and environmental water samples collected from the Pearl River were analyzed with the optimized LPME method, the concentrations of 18 CPs ranged from 0.0237microgL(-1) (3,5-DCP) to 0.3623microgL(-1) (2,3,6-TCP).
采用气相色谱 - 质谱联用技术，研究了一种通过衍生化液相微萃取（LPME）测定水样中18种氯酚（CPs）的样品预处理方法。将衍生化试剂加入萃取溶剂中，使衍生化和萃取一步完成。通过优化萃取溶剂、衍生化试剂百分比、萃取时间、pH值和离子强度等参数，可实现18种CPs衍生物的高灵敏度检测。最佳方法的结果表明，校准范围为0.5至500μg L⁻¹，相对标准偏差（RSD）在1.75%至9.39%之间，CPs的检测限（LOD）为0.01至0.12μg L⁻¹。此外，将所提出的LPME方法与固相微萃取（SPME）结合纤维上衍生化技术进行了比较。结果表明两种方法的结果相当一致。此外，通过加标环境样品评估的LPME回收率为87.9%（3,5 - DCP）至114.7%（2,3,5,6 - TeCP），并采用优化的LPME方法对采集自珠江的环境水样进行分析，18种CPs的浓度范围为0.0237μg L⁻¹（3,5 - DCP）至0.3623μg L⁻¹（2,3,6 - TCP）。
