Quintás Guillermo, Moros Javier, Armenta Sergio, Garrigues Salvador, de la Guardia Miguel
University of Valencia, Department of Analytical Chemistry, Edifici Jeroni Muñoz, 50th Dr. Moliner, 46100 Burjassot, Valencia, Spain.
J AOAC Int. 2005 Mar-Apr;88(2):399-405.
A routine method based on Fourier transform infrared spectrometry was developed for the simultaneous determination of pirimicarb and endosulfan in commercially available pesticide formulations. The method is based on peak area absorbance measurements between 1362 and 1352 cm(-1), corrected with a baseline fixed at 1338 cm(-1), for pirimicarb and peak area absorbance measurements between 919 and 909 cm(-1) with a baseline fixed at 931 cm(-1) for endosulfan; chloroform solutions for analysis were obtained by direct dilution of emulsifiable concentrates or by solvent extraction from solid samples. Various extraction conditions and appropriate band selection were investigated, and interference studies were performed. Under the experimental conditions selected, limits of detection of 13 microg/g for pirimicarb and 150 microg/g for endosulfan were obtained that correspond to 0.13 and 1.6% (w/w), respectively, in commercial samples. Results from analyses of commercial samples by the developed method compared well with those obtained by a liquid chromatography reference method.
开发了一种基于傅里叶变换红外光谱法的常规方法,用于同时测定市售农药制剂中的抗蚜威和硫丹。该方法基于在1362至1352 cm(-1)之间的峰面积吸光度测量,以1338 cm(-1)处固定的基线进行校正来测定抗蚜威,以及在919至909 cm(-1)之间的峰面积吸光度测量,以931 cm(-1)处固定的基线进行校正来测定硫丹;用于分析的氯仿溶液通过直接稀释乳油或从固体样品中进行溶剂萃取获得。研究了各种萃取条件和合适的谱带选择,并进行了干扰研究。在所选择的实验条件下,抗蚜威的检测限为13 μg/g,硫丹的检测限为150 μg/g,在商业样品中分别对应于0.13%和1.6%(w/w)。用所开发方法对商业样品的分析结果与液相色谱参考方法获得的结果相当。