Determination of 116 Pharmaceuticals and Personal Care Products in Water by Ultra‐High Performance Liquid Chromatography‐Tandem Mass Spectrometry

ABSTRACT This study examined an improved and simplified method for solid‐phase extraction that provides rapid and accurate determination and identification of 116 pharmaceutical and personal care products (PPCPs) in an aqueous environment using ultra‐high performance liquid chromatography‐tandem mass spectrometry. The common active compounds include 22 sulfonamides, 18 quinolones, 8 macrolides, 18 β‐agonists, 6 sedative‐hypnotics, 3 antipyretic‐analgesics, 3 antihypertensives, 2 antidiabetic drugs, 3 antihistamines, 8 sex hormones, 2 antivirals, 6 nitroimidazoles, 8 glucocorticoids, and 3 amphenicols, lincomycin, pimaricin, levothyroxine sodium, bisphenol A, aldosterone, and melamine in water samples. Key parameters of tandem mass spectrometry, ultra‐high performance liquid chromatography, and solid‐phase extraction were optimized to enhance the analytical performance. The calibration curves were accomplished at seven concentration levels, and a satisfactory linear relationship ( R > 0.99) was observed within the range of 5–800 ng/mL. Results showed varying limits of detection (0.0136–13.3 ng/L for different analytes based on signal‐to‐noise (S/N) = 3) and limits of quantitation (0.0452–44.4 ng/L). Recoveries of the spiked samples ranged from 53.1% to 116.5% with relative standard deviation lower than 9.9%. This approach effectively minimized matrix interference, improved extraction efficiency, and enhanced detection sensitivity, enabling more accurate PPCP residue analysis in water. The validated method was applied to raw water, treated water, and river water samples from Hangzhou, detecting 47 compounds at concentrations ranging from nondetected to 359 ng/L. Our findings provided critical technical support for the preliminary establishment of an environmental monitoring system targeting emerging pollutants. Notably, to the best of our knowledge, this study represented the first reported detection of melamine, loratadine, aldosterone, and levothyroxine sodium in aquatic environments. In particular, melamine was detected in aquatic environment for the first time, thus expanding the understanding of PPCPs’ pollution status.