This paper reports on the study for determination of Methamphetamine in urine samples by GC-MS method using Solid Phase (SPE). The aim of the study was investigation on the GC-MS method for determination of Methamphetamine in urine samples. The method is based on the extraction of Methamphetamine by using of Solid Phase Extraction technique with C18 and its determination by GC-MS. The method was then successfully applied for the determination of Methamphetamine in real samples.