An analytical method has been developed for the quantitative evaluation of 64 pharmaceuticals and personal care products in urban wastewater using solid‐phase extraction coupled with liquid chromatography‐tandem mass spectrometry. Design of experiments approach was used in the multiparametric optimization of solid‐phase extraction method for the analysis of pharmaceuticals and personal care products. The method was found to be linear within the range of 0.01–1 μg/L with coefficient of determination (R2) ranging from 0.990 to 0.999. The limit of detection and limit of quantification were found to be in the range of 0.002–0.028 and 0.007–0.091 μg/L, respectively. The accuracy was calculated with respect to percent recovery, and it was found to be in the range of 70.0–129% for all the analytes. The intra‐ and interday precisions were found to be less than 15% relative standard deviation for all the analytes. The developed analytical method was applied to real samples collected from four different sampling sites of Musi River in Hyderabad to evaluate its performance. The method found a wide application for the analysis of urban wastewater samples.

Prenylamine was initially used for the treatment of angina pectoris and later on withdrawn from the market in 1988 due to cardiac arrhythmias concern. The major phase I metabolite of prenylamine is p-hydroxy prenylamine that has a chiral center in the structure. Even though p-hydroxy prenylamine was synthesized earlier, it lacked complete analytical developments for chiral high-performance liquid chromatography (HPLC) separation. However, p-hydroxy prenylamine reference material is not commercially available. The innovation of this manuscript is the development and validation of a chiral HPLC separation method and more extensive characterization of the reference material than previously reported method. Therefore, it was hypothesized to develop and validate normal phase HPLC method for p-hydroxy prenylamine reference material. p-Hydroxy prenylamine was synthesized in two batches and characterized successfully using 13 C NMR, 1 H NMR, high-resolution mass spectrometry (HRMS), Fourier transform infrared spectroscopy (FT-IR), and thermogravimetric analysis (TGA). A normal phase chiral HPLC method was developed to analyze the p-hydroxy prenylamine purity. Separation of the p-hydroxy prenylamine enantiomers were achieved using ultra-high-performance liquid chromatography (UHPLC) on a ChiralCel ODH column at wavelength of 220 nm. The developed method was validated in terms of its linearity, accuracy, precision, and robustness for purification, purity assessment, and stability studies. Proton and carbon peaks were confirmed by nuclear magnetic resonance (NMR) analysis. Functional groups were confirmed by FT-IR. Loss on drying was 0.3% and 0.6% for Batches 1 and 2, respectively. The purity of the developed reference material for Batches 1 and 2 was found to be 99.59% and 100%, respectively. Therefore, the synthesized batches of p-hydroxy prenylamine can be used in dope testing as reference material.