Abstract
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 wastewater networks.
Highlights
The opioid epidemic is widespread in the US, causing nearly 450,000 overdose deaths since 1999 [1]
This study develops and validates a high performance liquid chro matography - tandem mass spectrometry method tailored to a panel of opioids including eight glucuronide conjugates: acetaminophen glucu ronide, codeine-6-glucuronide, hydromorphone-3-glucuronide, morphine-3-glucuronide, norbuprenorphine glucuronide, naloxone-3glucuronide, oxymorphone-3-glucuronide and (±)-11-nor-9-carboxydelta9-to estimate human consumption of cannabis (THC) glucuronide
If the observed concentration in an unknown sample falls above the upper limit, the sample is diluted to an appropriate level, spiked again with internal standards and reanalyzed by the instrument
Summary
The opioid epidemic is widespread in the US, causing nearly 450,000 overdose deaths since 1999 [1]. Each wave of the epidemic ushers in more fatal and non-fatal overdoses. Estimates of the intensity of each wave are based on first responder reports and hospital records. Unfor tunately, compiling these types of data can take a matter of years. Individuals who experience non-fatal opioid overdoses may never actively seek medical care [2,3]. These hidden populations suffering from opioid use disorder may benefit from empirically proven
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