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首页> 外文期刊>Fresenius' Journal of Analytical Chemistry >A multiresidue method with mobile on-site sampling based on SPE for ultratrace analysis of plant protectants in environmental waters
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A multiresidue method with mobile on-site sampling based on SPE for ultratrace analysis of plant protectants in environmental waters

机译:基于SPE的移动现场采样多残留方法用于环境水中植物保护剂的超痕量分析

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摘要

A new multiclass/multiresidue method for monitoring plant protectant residues in raw- and drinking waters with on-site sampling using a mobile, self-contained sampling unit based on SPE was developed and validated. 38 active compounds with widely varying chemical and physicochemical properties (acid-based properties, polarities, vapor pressures, solubilities) are measured from just one sample and work-up. 100 mL water, acidified with acetic acid, are drawn through a cartridge filled with Amberchrom resins by means of a calibrated 100 mL syringe driven by servo motors, control circuit and rechargeable battery. volumetric flow is high, quantitative extraction of acidic, neutral and weak basic substances is accomplished in a few minutes and loaded cartridges are transported into the laboratory. Further work-up, i.e. elution, drying, concentration and solvent change, is designed strictly non-selectively and produces 250 #mu#L of an "extract", which is the starting point of two GC measurement lines, GC-NPD and GC-ECD. Chlorinated herbicide acids are derivatised into perfluorinated benzyl esters employing reaction conditions so smooth that the organochlorine hydrocarbons are not destroyed at all and both substance classes can be chromatographed in one GC run. ECD-chromatograms from derivatised solutions are rather complex, therefore the flow is split after injection onto two columns with different polarities and two EC-detectors in order to resolve all analytes and matrix interferents. Short-chain carbonic acids added to the water prior to preconcentration are adsorbed on the hydrophobic surface in a reversible process and impart the Amberchrom resins with a partially hydrophilic character. Method performance was ascertained using tap water fortified at the 0.2 #mu#g L~(-1) level: Mean recoveries were between 70 and 115% and method detection limits (MDLs) below 0.08 #mu#g L~(-1). Waters from different sources did not affect the recoveries, loaded cartridges are stable for two weeks' storage when cooled.
机译:开发并验证了一种新的多类/多残留方法,该方法通过使用基于SPE的移动式自足式采样装置进行现场采样,可以监测原水和饮用水中植物保护剂的残留量。仅从一个样品就进行了38种活性化合物的化学和物理化学性质(基于酸的性质,极性,蒸气压,溶解度)的变化测量。借助由伺服电机,控制电路和可充电电池驱动的经过校准的100 mL注射器,将100 mL用乙酸酸化的水从装有Amberchrom树脂的药筒中抽出。体积流量很高,可在几分钟内完成对酸性,中性和弱碱性物质的定量提取,并将已装载的药筒运输到实验室。严格非选择性地设计了进一步的处理方法,即洗脱,干燥,浓度和溶剂变化,并产生了250#mu#L的“提取物”,这是两条GC测量线GC-NPD和GC的起点-ECD。采用平滑的反应条件将氯化的除草剂酸衍生为全氟苄基酯,以至于有机氯烃完全不被破坏,并且两种物质都可以在一次GC中进行色谱分离。衍生溶液的ECD色谱图非常复杂,因此,在进样后,将流量分成两根极性不同的色谱柱和两个EC检测器,以分离所有分析物和基质干扰物。在预浓缩之前添加到水中的短链碳酸可逆地吸附在疏水表面上,使Amberchrom树脂具有部分亲水性。使用浓度为0.2#mu#g L〜(-1)的自来水确定方法性能:平均回收率在70%至115%之间,方法检测限(MDL)低于0.08#mu#g L〜(-1) 。来自不同水源的水不会影响回收率,冷却后,装载的滤芯可以稳定存放两个星期。

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