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The importance of the role of analysis of herbicides and other toxic substances in environmental and food samples, toxicology, environmental research and health related discipline is self-evident. Analytical methods are required by various regularity agencies, for validation, which requires the demonstration of the specificity, sensitivity, calibration linearity, extraction recovery, precision and accuracy of the assay method. The aim of present study was to develop new Spectrophotometric and HPLC methods for the determination of dinitroaniline and aryloxyphenoxy group of herbicides in various environmental and agricultural samples.