Chemical fingerprinting and quantitative monitoring of the doping drugs bambuterol and terbutaline in human urine samples using ATR-FTIR coupled with a PLSR chemometric tool

Abstract

The use of performance-enhancing drugs is prohibited in sports competitions according to the World Anti-Doping Agency (WADA) regulations. Here, ATR-FTIR spectroscopy coupled with a partial least squares regression (PLSR) chemometric tool was used for the detection of the misuse of such substances. Bambuterol and its metabolite terbutaline have been included in the list of prohibited doping agents. Therefore, we used bambuterol and terbutaline as models for the accurate and simultaneous qualitative and quantitative analysis of bambuterol and terbutaline in human urine samples. The method was straightforward and once the urine samples were collected, they could be directly applied to the surface of the ZnSe prism (ATR unit) to get the results within one minute. A calibration set with a partial factorial design was used to develop the PLSR model that could be used to predict the concentration of unknown samples containing the two drugs. The developed method was carefully validated and successfully applied to the urine sample analysis of human volunteers. The drugs were quantified at nanogram level concentrations. A side-by-side comparison of the proposed method with the routine GC-MS method was performed to demonstrate the challenges and opportunities of each method.