Zhang Jie, Lee Hian Kee
Department of Chemistry, National University of Singapore, 3 Science Drive 3, Singapore 117543, Singapore.
J Chromatogr A. 2006 Jun 2;1117(1):31-7. doi: 10.1016/j.chroma.2006.03.102. Epub 2006 Apr 19.
A method has been established for the determination of five carbamate pesticides in water samples using liquid-phase microextraction (LPME) followed by on-column derivatization and gas chromatography-mass spectrometric (GC-MS) determination. Trimethylphenylammonium hydroxide (TMPAH) and trimethylsulfonium hydroxide (TMSH) were used as derivatization reagent for extracts prior to GC-MS analysis as carbamate pesticides are thermally labile compounds. Parameters that affect the extraction efficiency (selection of organic solvent and extraction time) and derivatization efficiency (choice of derivatization reagent and concentration of derivatization reagent) were investigated. The proposed method provided good enrichment factors up to 224, with reproducibility ranging from 4.86 to 7.81%, and good linearity from 1 to 400 microg/L. The limits of detection (LODs) ranged between 0.2 and 0.8 microg/L (S/N = 3) using GC-MS with selective ion monitoring. This method was applied to the determination of carbamate pesticides in tap water and waste water.
已建立一种采用液相微萃取（LPME）、柱上衍生化和气相色谱-质谱联用（GC-MS）测定法来测定水样中5种氨基甲酸酯类农药的方法。由于氨基甲酸酯类农药是热不稳定化合物，在GC-MS分析之前，使用氢氧化三甲基苯基铵（TMPAH）和氢氧化三甲基锍（TMSH）作为提取物的衍生化试剂。研究了影响萃取效率（有机溶剂的选择和萃取时间）和衍生化效率（衍生化试剂的选择和衍生化试剂的浓度）的参数。所提出的方法提供了高达224的良好富集因子，重现性范围为4.86%至7.81%，线性良好，范围为1至400μg/L。使用GC-MS选择性离子监测时，检测限（LOD）在0.2至0.8μg/L之间（S/N = 3）。该方法应用于自来水和废水中氨基甲酸酯类农药的测定。
