Analysis of 39 drugs and metabolites, including 8 glucuronide conjugates, in an upstream wastewater network via HPLC-MS/MS

Abstract

© The Author(s), 2021. This article is distributed under the terms of the Creative Commons Attribution License. The definitive version was published in Foppe, K. S., Kujawinski, E. B., Duvallet, C., Endo, N., Erickson, T. B., Chai, P. R., & Matus, M. Analysis of 39 drugs and metabolites, including 8 glucuronide conjugates, in an upstream wastewater network via HPLC-MS/MS. Journal of Chromatography B, 1176, (2021): 122747, https://doi.org/10.1016/j.jchromb.2021.122747.Pharmaceutical compounds ingested by humans are metabolized and excreted in urine and feces. These metabolites can be quantified in wastewater networks using wastewater-based epidemiology (WBE) methods. Standard WBE methods focus on samples collected at wastewater treatment plants (WWTPs). However, these methods do not capture more labile classes of metabolites such as glucuronide conjugates, products of the major phase II metabolic pathway for drug elimination. By shifting sample collection more upstream, these unambiguous markers of human exposure are captured before hydrolysis in the wastewater network. In this paper, we present an HPLC-MS/MS method that quantifies 8 glucuronide conjugates in addition to 31 parent and other metabolites of prescription and synthetic opioids, overdose treatment drugs, illicit drugs, and population markers. Calibration curves for all analytes are linear (r2 > 0.98), except THC (r2 = 0.97), and in the targeted range (0.1–1,000 ng mL−1) with lower limits of quantification (S/N = 9) ranging from 0.098 to 48.75 ng mL−1. This method is fast with an injection-to-injection time of 7.5 min. We demonstrate the application of the method to five wastewater samples collected from a manhole in a city in eastern Massachusetts. Collected wastewater samples were filtered and extracted via solid-phase extraction (SPE). The SPE cartridges are eluted and concentrated in the laboratory via nitrogen-drying. The method and case study presented here demonstrate the potential and application of expanding WBE to monitoring labile metabolites in upstream wastewaterThis work was supported by the National Institute on Drug Abuse of the National Institutes of Health award number R44DA051106 to MM and PC. TE, PC and MM are funded by research grants from the Massachusetts Consortium on Pathogen Readiness and NIH R44DA051106. PRC is funded by NIH K23DA044874, independent research grants from e-ink corporation and Hans and Mavis Lopater Psychosocial Foundation