竹炭固相萃取-分散液相微萃取-气相色谱/质谱检测水中酰胺类除草剂

Solid-Phase Extraction based on Bamboo-charcoal Followed by Dispersive Liquid Liquid Microextraction for Determination of Amide Herbicides in Water Samples by GC/MS

建立了一种新型、灵敏的检测水中酰胺类除草剂的分析方法。以固相萃取结合分散液相微萃取作为预处理技术,利用气相色谱/质谱检测酰胺类除草剂。优化了洗脱剂种类、流速、水样体积及pH值、盐效应等实验条件。在优化实验条件下,方法的检出限为0.16~1.12 ng·L-1,甲草胺、乙草胺和丁草胺的线性范围分别为2.0~104 ng·L-1,5.0~104 ng·L-1和1.0~104 ng·L-1。将所建立的方法用于河水和水库水中酰胺类除草剂的检测,加标回收率为76.6%~93.5%,结果满意。

A novel and sensitive approach based on solid phase extraction（SPE） followed by dispersive liquid liquid microextraction（DLLME） for determination of trace amide herbicides in environmental water samples prior to gas chromatography/mass spectrometry（GC/MS） was proposed. Key parameters such as kind of eluant, sample flow rate, volume and pH of water samples, salt addition were all investigated in detail. On the optimum conditions, limits of detection were in the range of 0.16-1.12 ng·L^-1, depending on the analytes. The calibration curves were linear in the range of 2.0-104 ng·L^-1 for alachlor, 5.0-104 ng·L^-1 for acetochlor, and 1.0-104 ng·L^-1 for butachlor, respectively. The novel method was successfully applied to the analysis of the three amide herbicides in river water and reservoir water samples with the relative recoveries in the range between 76.6 % and 93.5 % at spiking level of 50.0 ng L^-1 and a satisfactory result was obtained.