Many of the challenges posed by the quantitative analysis of drug candidates in biological fluids are met by atmospheric pressure ionization tandem mass spectrometry (MS/MS). However, the development of suitable methodology requires the determination and optimization of many compound-specific instrumental variables. At a minimum, the m/z values of a precursor ion and a product ion, along with the optimum collision energy, must be known in order to construct a suitable method. MS/MS method performance is particularly sensitive to collision energy, which must be near-optimum for each compound analysed. Conventionally, these instrumental parameters are determined by continuous infusion of a standard solution into the ion source and optimizing each individual parameter. This paper describes the application of a technique based on the triple quadrupole mass spectrometer which streamlines the development of quantitative MS/MS methods. Termed a Q3 CID (collision-induced dissociation) scan, the method involves collection of Q3 spectra with a pressurized collision cell and flow injection sample introduction. Operation in this mode introduces all precursor ions into the collision cell, eliminating the need to perform multiple manual experiments. Data are presented which demonstrate that the majority of the information required to construct an MS/MS quantitation method can be obtained in a single flow-injection experiment. Performance of quantitative methods constructed with instrument parameters gathered from positive-ion Q3 CID, compared with that of methods developed using conventional infusion optimization is presented. Limitations and applications particular to bioanalytical quantitation are discussed.