This paper demonstrates headspace liquid-phase microextraction (HS-LPME) as used for the determination of volatile residual solvents in pharmaceutical products. This method is based on headspace liquid-phase microextraction capillary column gas chromatography. Under optimum conditions, the linerary of the method ranged from 1 to 1,000 mg l(-1). The limits of detection are 0.2-6.0 [corrected] mg l(-1) and relative standard deviations (RSD) for most of the volatile solvents were below 10%. This novel method is applied to the analysis of volatile residual solvents in pharmaceutical products with satisfactory results.