OBJECTIVE: Simulateous determination of ten psychosedatives in serum was made to help doctors make effective rescue. METHOD: The qualitative separation was done by TLC. The quantitative determination was made by TLC scanning. RESULTS: Ten psychosedatives were separated very well by one mobile phase. The recovery, accuracy and stability of TLC scanning on varied wave-lengths were satisfatory. CONCLUSION: This method is simple, rapid, and accurate. It can be used in poison analysis and therapeutic drug monitoring.