Development of a pH-paralleling approach of quantifying six-category pharmaceuticals in surface water using SPE-HPLC-MS/MS

Abstract

An analytical protocol was developed to quantify six-category pharmaceuticals in surface water under paralleling pHs using a combination of solid phase extraction (SPE) and high-performance liquid chromatography tandem mass spectrometry (HPLC-MS/MS). Of 121 compound standards commercially, 94 compounds were reliably quantified using a paralleling pH combination at 3 and 9 with a sound recovery-rate of 50-150%. The quantified compounds covered 6 categories as 37 antibiotics, 16 central nervous system drugs (CNs), 14 cardiovascular drugs (CVs), 12 endocrine and family planning drugs (EFs), 8 antiparasitic drugs (APs), and 7 non-steroidal anti-inflammatory drugs (NSAIDs). The protocol achieved limits of detection and quantitation in ranges of 0.001–11.9 ng L^–1 and 0.003–39.7 ng L^–1, respectively. Serial field surface water samples from Jiulong River in Fujian, China were testified using the protocol with 41 quantified compounds of the above-mentioned 6 categories from < LODs to 1,389 ng L⁻¹ (caffeine). The key procedure prior to the SPE is to split filtrate of each surface water sample into two portions, adjusted to pH 3 and 9 separately and both spiked with 0.2 g Na₂EDTA.