11-nor-9-Carboxy-THC, also known as THCA or carboxy-THC, is the main secondary metabolite of THC (the active component of marijuana) formed in the human body [1]. THCA is excreted in urine in the form of glucuronide conjugates. THCA is not psychoactive but has a long half-life of up to several days or even weeks in very heavy users, thus determination of THCA in urine plays an important role in confirmation of marijuana consumption. The Substance Abuse and Mental Health Services Administration (SAMHSA) has set the THCA cutoff concentration of confirmatory testing at 15 ng/mL. Typical sample preparation methods for THCA in urine include liquid-liquid extraction (LLE) and solid phase extraction (SPE). This application utilizes a novel sample preparation technique, QuEChERS to effectively quantitate THCA levels in human urine.