In this work an automated DPX procedure is presented that enables the determination of acidic, basic, and neutral drugs in small blood or urine samples. The DPX method is based on a mixed-mode cation exchange sorbent (CX) with reversed phase characteristics. The automated extraction is shown to require only minimal manual labor when performed using the GERSTEL MPS 2 autosampler under MAESTRO software control. GC-MS data is provided showing that comprehensive, rapid and sensitive analysis can be performed using automated DPX combined with large volume injection. Automated sample preparation steps are performed during the GC/MS run of the preceding sample using the MAESTRO PrepAhead function. PrepAhead sample preparation enables high throughput analysis, improved productivity and “just in time” preparation of each sample.