This study features the simultaneous extraction and quantification of 18 pharmaceuticals and personal care products (PPCPs). This is a pioneering method for the quantification of acetaminophen, sulfamethoxazole, diclofenac, atenolol, metoprolol, diethyltoluamide and oxybenzone in atmospheric pressure chemical ionisation mode. The method was validated for high repeatability and reproducibility with relative standard deviations less than 10%. Instrument quantification limits for PPCPs were within the range of 0.05–1.0 µg L−1, and the method quantification limits (MQLs) for ultrapure water were within the range of 0.3–15 ng L−1. All samples were extracted using Oasis© hydrophilic–lipophilic balanced cartridges with optimised sample size and extraction conditions. Good accuracy was demonstrated, with solid-phase extraction recoveries above 80% for most PPCPs. In environmental matrices, the MQLs for river water, sewage treatment plant (STP) effluent and STP influent were 4–25, 10–153 and 38–386.5, respectively. The method was successfully applied to investigate occurrences of persistent PPCPs in Malaysian river and sewage samples.