The objective of this research to optimise the HPLC method was developed for quantitative determination of Pirimiphos-methyl. Chromatographic separation was achieved on a 250 x 4.6 mm i.d. reversed phase column Qualisil BDS 5u C18, Using deionized acetonitrile:water in the ratio of 85:15 v/v respectively as mobile phase. The eluent was monitored at 254 nm. A sharp peak was obtained for the Pirimiphos-methyl at 9.29 min. The UV Spectrophotometric method performed at 254 nm after full scan analysis using methanol as a solvent. The result revealed that both methods are suitable to carry out routine analysis of Pirimiphos methyl, However HPLC results showed high precise, accurate and sensitive than the UV Spectrophotometer. Hence HPLC method is suitable for trace analysis of Pirimiphos methyl in environmental samples.