Mrabet K El, Poitevin M, Vial J, Pichon V, Amarouche S, Hervouet G, Lalere B
Laboratoire Environnement et Chimie Analytique, Ecole Supérieure de Physique et Chimie Industrielles de la Ville de Paris, 10 Rue Vauquelin, 75005 Paris, France.
J Chromatogr A. 2006 Nov 17;1134(1-2):151-61. doi: 10.1016/j.chroma.2006.08.100. Epub 2006 Oct 12.
Matrix reference materials (MRM) are essential tools for the validation of analytical protocols. Nowadays, there are no such materials for the determination of herbicides in water. Pesticides stored in acetonitrile and stored on solid phase extraction (SPE) cartridges previously percolated with a water sample spiked with triazines and phenylureas have proven to be good candidates for reference materials because of their satisfactory stability under appropriate temperature conditions. To evaluate the behaviors of these materials containing pesticides and to be analyzed by liquid chromatography, a collaborative study including 15 laboratories has been organized. Observed reproducibility on candidate materials after the removal of extreme results was 16.1% for the vials with pesticides in acetonitrile (at around 0.125 mg/L) directly analyzed, 29.2% for a water sample spiked with the pesticides (at around 0.5 microg/L) analyzed after preconcentration on a cartridge and 26.7% for the cartridges previously percolated with a water containing the pesticides (250 mL at around 0.5 microg/L for each pesticide) analyzed after elution. Such dispersion values are quite compatible with the requirement of a further certification for such materials.
基质参考物质（MRM）是分析方法验证的重要工具。目前，尚无用于测定水中除草剂的此类物质。储存在乙腈中并储存在先前用加有三嗪和苯基脲的水样渗滤过的固相萃取（SPE）小柱上的农药，由于在适当温度条件下具有令人满意的稳定性，已被证明是很好的参考物质候选物。为了评估这些含农药物质的行为并通过液相色谱进行分析，组织了一项包括15个实验室的协同研究。去除极端结果后，直接分析的含乙腈中农药的小瓶（浓度约为0.125 mg/L）的候选物质的观察重现性为16.1%，在小柱上预浓缩后分析的加有农药的水样（浓度约为0.5 μg/L）的重现性为29.2%，先前用含农药的水（每种农药约0.5 μg/L的250 mL）渗滤过的小柱洗脱后分析的重现性为26.7%。这样的分散值与对此类物质进一步认证的要求相当相符。
