采用HPLC-FLD放大测量草甘膦浓度的方法

Natalya E. Fedorova, A. A. Ivchenkova, Nataliya Andreevna Stepanova, S. D. Dobrev
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摘要

介绍。传统上,当使用草甘膦制剂(一种世界上非常流行的除草剂)时,对工作条件的卫生评估是基于薄层色谱法的使用。本文考虑了几种替代方法。在实验数据的基础上,优化了高效液相色谱法分析空气中草甘膦含量的条件。材料和方法。所有使用草甘膦溶液的工作都在聚丙烯容器中进行。在介质过滤过滤器(“蓝带”)上对空气介质进行采样。随后用水提取。采用高效液相色谱法,荧光检测器,激发波长为270 nm,发射波长为313 nm。用9-氟酰氯甲酸甲酯在碱性介质中衍生化草甘膦后,用甲苯加热并洗去过量的试剂,将草甘膦转化为具有荧光特性的分子。采用C18反相色谱柱;以乙酸铵加乙酸和乙腈为洗脱剂。结果。采用草甘膦制剂对休耕地和工业地区土地进行地面处理时取得的实际样品对所开发的技术进行了批准。检测到的草甘膦含量均未超过定量检测下限:工作区空气中草甘膦含量为0.5 mg/m3,大气中草甘膦含量为0.025 mg/m3(最大允许浓度分别为1.0和0.1 mg/m3)。的局限性。该研究考虑了有限数量的色谱柱。对25个工作区域空气和大气空气的模型样本进行了研究。结论。根据所执行的工作结果,形成了“用高效液相色谱法测量空气中草甘膦浓度”的方法说明,并以批准的方式发送计量认证。
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Methodical approaches to scale-up measurement of glyphosate concentration using HPLC-FLD
Introduction. Traditionally, the hygienic assessment of working conditions when using glyphosate preparations, an extremely popular herbicide in the world, is based on the use of thin layer chromatography. In this paper, alternative approaches are considered. On the basis of experimental data, the conditions for the analysis of glyphosate content in air by high performance liquid chromatography were optimized. Material and methods. All work with glyphosate solutions was carried out in polypropylene vessels. Sampling from the air medium was carried out on a medium filtration filter (“blue ribbon”). Subsequent extraction was carried out with water. The measurements were performed by high performance liquid chromatography with a fluorimetric detector at an excitation wavelength of 270 nm and an emission wavelength of 313 nm. To transfer glyphosate to a molecule with fluorimetric properties after derivatization of glyphosate in an alkaline medium using 9-fluorenylmethyl chloroformate by heating and washing off the excess of the reagent with toluene. A C18 reverse phase column was used; ammonium acetate with the addition of acetic acid and acetonitrile were used as eluents. Results. Approbation of the developed technique was carried out on real samples taken during ground treatment of fallow fields and lands of industrial territories with glyphosate preparations. The detected levels of glyphosate did not exceed the lower limit of quantitative determination: 0.5 mg/m3 in the air of the working area and 0.025 mg/m3 in the atmospheric air (with maximum allowable concentrations of 1.0 and 0.1 mg/m3, respectively). Limitations. The study considers a limited number of chromatographic columns. The study is performed on 25 model samples of the air of the working area and atmospheric air. Conclusion. Based on the results of the work performed, methodological instructions “Measurement of glyphosate concentrations in the air by high-performance liquid chromatography” were formed and sent for metrological certification in the approved manner.
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