USP Residual Solvents is a general chapter in the US Pharmacopeia that describes a headspace gas chromatographic method for the determination of residual solvents in pharmaceutical products, active ingredients, and excipients. As originally written, it described parameters used with balanced-pressure or pressure loop based headspace instruments. Recent updates have included parameters for syringe based systems. This application note demonstrates implementation of USP Residual Solvents using the GERSTEL MPS 2 configured as automated headspace sampler. Children’s non-aspirin (acetaminophen) suspension liquid was purchased locally and spiked to a level of 2000 μg/g (5 times the acceptable concentration limit) with acetonitrile.