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

Foppe, Katelyn S / Kujawinski, Elizabeth B / Duvallet, Claire / Endo, Noriko / Erickson, Timothy B / Chai, Peter R / Matus, Mariana

Journal of chromatography. 2021 June 30, v. 1176

2021

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 ... ...

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.
Keywords	biochemical pathways ; case studies ; chemical species ; drug excretion ; epidemiology ; feces ; humans ; hydrolysis ; metabolites ; narcotics ; overdose ; solid phase extraction ; urine ; wastewater ; wastewater treatment ; Massachusetts
Language	English
Dates of publication	2021-0630
Publishing place	Elsevier B.V.
Document type	Article
ISSN	1570-0232
DOI	10.1016/j.jchromb.2021.122747
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Article ; Online: Mapping Community Opioid Exposure Through Wastewater-Based Epidemiology as a Means to Engage Pharmacies in Harm Reduction Efforts.

Duvallet, Claire / Hayes, Bryan D / Erickson, Timothy B / Chai, Peter R / Matus, Mariana

Preventing chronic disease

2020 Volume 17, Page(s) E91

MeSH term(s)	Analgesics, Opioid/pharmacokinetics ; Community Pharmacy Services/organization & administration ; Harm Reduction ; Humans ; North Carolina ; Opioid Epidemic ; Opioid-Related Disorders/prevention & control ; Pilot Projects ; Wastewater-Based Epidemiological Monitoring
Chemical Substances	Analgesics, Opioid
Language	English
Publishing date	2020-08-20
Publishing country	United States
Document type	Journal Article
ZDB-ID	2135684-1
ISSN	1545-1151 ; 1545-1151
ISSN (online)	1545-1151
ISSN	1545-1151
DOI	10.5888/pcd17.200053
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Article ; Online: "Waste Not, Want Not" - Leveraging Sewer Systems and Wastewater-Based Epidemiology for Drug Use Trends and Pharmaceutical Monitoring.

Erickson, Timothy B / Endo, Noriko / Duvallet, Claire / Ghaeli, Newsha / Hess, Kaitlyn / Alm, Eric J / Matus, Mariana / Chai, Peter R

Journal of medical toxicology : official journal of the American College of Medical Toxicology

2021 Volume 17, Issue 4, Page(s) 397–410

Abstract: During the current global COVID-19 pandemic and opioid epidemic, wastewater-based epidemiology (WBE) has emerged as a powerful tool for monitoring public health trends by analysis of biomarkers including drugs, chemicals, and pathogens. Wastewater ... ...

Abstract	During the current global COVID-19 pandemic and opioid epidemic, wastewater-based epidemiology (WBE) has emerged as a powerful tool for monitoring public health trends by analysis of biomarkers including drugs, chemicals, and pathogens. Wastewater surveillance downstream at wastewater treatment plants provides large-scale population and regional-scale aggregation while upstream surveillance monitors locations at the neighborhood level with more precise geographic analysis. WBE can provide insights into dynamic drug consumption trends as well as environmental and toxicological contaminants. Applications of WBE include monitoring policy changes with cannabinoid legalization, tracking emerging illicit drugs, and early warning systems for potent fentanyl analogues along with the resurging wave of stimulants (e.g., methamphetamine, cocaine). Beyond drug consumption, WBE can also be used to monitor pharmaceuticals and their metabolites, including antidepressants and antipsychotics. In this manuscript, we describe the basic tenets and techniques of WBE, review its current application among drugs of abuse, and propose methods to scale and develop both monitoring and early warning systems with respect to measurement of illicit drugs and pharmaceuticals. We propose new frontiers in toxicological research with wastewater surveillance including assessment of medication assisted treatment of opioid use disorder (e.g., buprenorphine, methadone) in the context of other social burdens like COVID-19 disease.
MeSH term(s)	Biomarkers/analysis ; COVID-19/epidemiology ; Humans ; Illicit Drugs/analysis ; Pandemics ; Pharmaceutical Preparations/analysis ; SARS-CoV-2 ; Substance Abuse Detection/methods ; Substance-Related Disorders/epidemiology ; Wastewater/chemistry ; Wastewater-Based Epidemiological Monitoring ; Water Pollutants, Chemical/analysis
Chemical Substances	Biomarkers ; Illicit Drugs ; Pharmaceutical Preparations ; Waste Water ; Water Pollutants, Chemical
Language	English
Publishing date	2021-08-16
Publishing country	United States
Document type	Journal Article ; Research Support, N.I.H., Extramural
ZDB-ID	2435016-3
ISSN	1937-6995 ; 1556-9039
ISSN (online)	1937-6995
ISSN	1556-9039
DOI	10.1007/s13181-021-00853-4
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Article ; Online: Analysis of 39 drugs and metabolites, including 8 glucuronide conjugates, in an upstream wastewater network via HPLC-MS/MS.

Foppe, Katelyn S / Kujawinski, Elizabeth B / Duvallet, Claire / Endo, Noriko / Erickson, Timothy B / Chai, Peter R / Matus, Mariana

Journal of chromatography. B, Analytical technologies in the biomedical and life sciences

2021 Volume 1176, Page(s) 122747

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 (r
MeSH term(s)	Chromatography, High Pressure Liquid/methods ; Glucuronides/analysis ; Limit of Detection ; Linear Models ; Pharmaceutical Preparations/analysis ; Reproducibility of Results ; Tandem Mass Spectrometry/methods ; Wastewater/chemistry ; Water Pollutants, Chemical/analysis
Chemical Substances	Glucuronides ; Pharmaceutical Preparations ; Waste Water ; Water Pollutants, Chemical
Language	English
Publishing date	2021-05-13
Publishing country	Netherlands
Document type	Journal Article
ZDB-ID	1180823-8
ISSN	1873-376X ; 0378-4347 ; 1570-0232 ; 1387-2273
ISSN (online)	1873-376X
ISSN	0378-4347 ; 1570-0232 ; 1387-2273
DOI	10.1016/j.jchromb.2021.122747
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Article ; Online: Rapid Assessment of Opioid Exposure and Treatment in Cities Through Robotic Collection and Chemical Analysis of Wastewater.

Endo, Norkio / Ghaeli, Newsha / Duvallet, Claire / Foppe, Katelyn / Erickson, Timothy B / Matus, Mariana / Chai, Peter R

Journal of medical toxicology : official journal of the American College of Medical Toxicology

2020 Volume 16, Issue 2, Page(s) 195–203

Abstract: Introduction: Accurate data regarding opioid use, overdose, and treatment is important in guiding community efforts at combating the opioid epidemic. Wastewater-based epidemiology (WBE) is a potential method to quantify community-level trends of opioid ... ...

Abstract	Introduction: Accurate data regarding opioid use, overdose, and treatment is important in guiding community efforts at combating the opioid epidemic. Wastewater-based epidemiology (WBE) is a potential method to quantify community-level trends of opioid exposure beyond overdose data, which is the basis of most existing response efforts. However, most WBE efforts collect parent opioid compounds (e.g., morphine) at wastewater treatment facilities, measuring opioid concentrations across large catchment zones which typically represent an entire municipality. We sought to deploy a robotic sampling device at targeted manholes within a city to semi-quantitatively detect opioid metabolites (e.g., morphine glucuronide) at a sub-city community resolution. Methods: We deployed a robotic wastewater sampling platform at ten residential manholes in an urban municipality in North Carolina, accounting for 44.5% of the total municipal population. Sampling devices comprised a robotic sampling arm with in situ solid phase extraction, and collected hourly samples over 24-hour periods. We used targeted mass spectrometry to detect the presence of a custom panel of opioids, naloxone, and buprenorphine. Results: Ten sampling sites were selected to be a representative survey of the entire municipality by integrating sewer network and demographic GIS data. All eleven metabolites targeted were detected during the program. The average morphine milligram equivalent (MME) across the nine illicit and prescription opioids, as excreted and detected in wastewater, was 49.1 (standard deviation of 31.9) MME/day/1000-people. Codeine was detected most frequently (detection rate of 100%), and buprenorphine was detected least frequently (12%). The presence of naloxone correlated with city data of known overdoses reversed by emergency medical services in the prehospital setting. Conclusion: Wastewater-based epidemiology with smart sewer selection and robotic wastewater collection is feasible to detect the presence of specific opioids, naloxone, methadone, and buprenorphine within a city. These results suggest that wastewater epidemiology could be used to detect patterns of opioid exposure and may ultimately provide information for opioid use disorder (OUD) treatment and harm reduction programs.
MeSH term(s)	Adult ; Analgesics, Opioid/analysis ; Environmental Monitoring/instrumentation ; Feasibility Studies ; Female ; Humans ; Male ; Mass Spectrometry ; Middle Aged ; Naloxone/analysis ; Narcotic Antagonists/analysis ; North Carolina ; Opioid Epidemic ; Opioid-Related Disorders/diagnosis ; Opioid-Related Disorders/epidemiology ; Opioid-Related Disorders/therapy ; Robotics/instrumentation ; Solid Phase Extraction ; Substance-Related Disorders/diagnosis ; Substance-Related Disorders/epidemiology ; Substance-Related Disorders/therapy ; Urban Health ; Waste Water/analysis ; Water Pollutants, Chemical/analysis
Chemical Substances	Analgesics, Opioid ; Narcotic Antagonists ; Waste Water ; Water Pollutants, Chemical ; Naloxone (36B82AMQ7N)
Language	English
Publishing date	2020-01-09
Publishing country	United States
Document type	Journal Article ; Research Support, N.I.H., Extramural ; Research Support, Non-U.S. Gov't
ZDB-ID	2435016-3
ISSN	1937-6995 ; 1556-9039
ISSN (online)	1937-6995
ISSN	1556-9039
DOI	10.1007/s13181-019-00756-5
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Article: Progressive Shifts in the Gut Microbiome Reflect Prediabetes and Diabetes Development in a Treatment-Naive Mexican Cohort.

Diener, Christian / Reyes-Escogido, María de Lourdes / Jimenez-Ceja, Lilia M / Matus, Mariana / Gomez-Navarro, Claudia M / Chu, Nathaniel D / Zhong, Vivian / Tejero, M Elizabeth / Alm, Eric / Resendis-Antonio, Osbaldo / Guardado-Mendoza, Rodolfo

Frontiers in endocrinology

2021 Volume 11, Page(s) 602326

Abstract: Type 2 diabetes (T2D) is a global epidemic that affects more than 8% of the world's population and is a leading cause of death in Mexico. Diet and lifestyle are known to contribute to the onset of T2D. However, the role of the gut microbiome in T2D ... ...

Abstract	Type 2 diabetes (T2D) is a global epidemic that affects more than 8% of the world's population and is a leading cause of death in Mexico. Diet and lifestyle are known to contribute to the onset of T2D. However, the role of the gut microbiome in T2D progression remains uncertain. Associations between microbiome composition and diabetes are confounded by medication use, diet, and obesity. Here we present data on a treatment-naive cohort of 405 Mexican individuals across varying stages of T2D severity. Associations between gut bacteria and more than 200 clinical variables revealed a defined set of bacterial genera that were consistent biomarkers of T2D prevalence and risk. Specifically, gradual increases in blood glucose levels, beta cell dysfunction, and the accumulation of measured T2D risk factors were correlated with the relative abundances of four bacterial genera. In a cohort of 25 individuals, T2D treatment-predominantly metformin-reliably returned the microbiome to the normoglycemic community state. Deep clinical characterization allowed us to broadly control for confounding variables, indicating that these microbiome patterns were independent of common T2D comorbidities, like obesity or cardiovascular disease. Our work provides the first solid evidence for a direct link between the gut microbiome and T2D in a critically high-risk population. In particular, we show that increased T2D risk is reflected in gradual changes in the gut microbiome. Whether or not these T2D-associated changes in the gut contribute to the etiology of T2D or its comorbidities remains to be seen.
MeSH term(s)	Bacteria/classification ; Bacteria/drug effects ; Bacteria/isolation & purification ; Case-Control Studies ; Cohort Studies ; Diabetes Mellitus, Type 2 ; Feces/microbiology ; Gastrointestinal Microbiome ; Humans ; Hypoglycemic Agents/therapeutic use ; Life Style ; Metformin/therapeutic use ; Mexico/epidemiology ; Prediabetic State/drug therapy ; Prediabetic State/epidemiology ; Prediabetic State/microbiology ; Prediabetic State/pathology ; Risk Factors
Chemical Substances	Hypoglycemic Agents ; Metformin (9100L32L2N)
Language	English
Publishing date	2021-01-08
Publishing country	Switzerland
Document type	Journal Article ; Research Support, Non-U.S. Gov't
ZDB-ID	2592084-4
ISSN	1664-2392
ISSN	1664-2392
DOI	10.3389/fendo.2020.602326
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Article ; Online: Wastewater network infrastructure in public health: Applications and learnings from the COVID-19 pandemic.

Sharara, Nour / Endo, Noriko / Duvallet, Claire / Ghaeli, Newsha / Matus, Mariana / Heussner, Jennings / Olesen, Scott W / Alm, Eric J / Chai, Peter R / Erickson, Timothy B

PLOS global public health

2021 Volume 1, Issue 12

Abstract: Accurate estimates of COVID-19 burden of infections in communities can inform public health strategy for the current pandemic. Wastewater based epidemiology (WBE) leverages sewer infrastructure to provide insights on rates of infection by measuring viral ...

Abstract	Accurate estimates of COVID-19 burden of infections in communities can inform public health strategy for the current pandemic. Wastewater based epidemiology (WBE) leverages sewer infrastructure to provide insights on rates of infection by measuring viral concentrations in wastewater. By accessing the sewer network at various junctures, important insights regarding COVID-19 disease activity can be gained. The analysis of sewage at the wastewater treatment plant level enables population-level surveillance of disease trends and virus mutations. At the neighborhood level, WBE can be used to describe trends in infection rates in the community thereby facilitating local efforts at targeted disease mitigation. Finally, at the building level, WBE can suggest the presence of infections and prompt individual testing. In this critical review, we describe the types of data that can be obtained through varying levels of WBE analysis, concrete plans for implementation, and public health actions that can be taken based on WBE surveillance data of infectious diseases, using recent and successful applications of WBE during the COVID-19 pandemic for illustration.
Language	English
Publishing date	2021-12-02
Publishing country	United States
Document type	Journal Article
ISSN	2767-3375
ISSN (online)	2767-3375
DOI	10.1371/journal.pgph.0000061
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Article: Metrics to relate COVID-19 wastewater data to clinical testing dynamics

Water research. 2022 Apr. 01, v. 212

2022

Abstract: Wastewater surveillance has emerged as a useful tool in the public health response to the COVID-19 pandemic. While wastewater surveillance has been applied at various scales to monitor population-level COVID-19 dynamics, there is a need for quantitative ... ...

Abstract	Wastewater surveillance has emerged as a useful tool in the public health response to the COVID-19 pandemic. While wastewater surveillance has been applied at various scales to monitor population-level COVID-19 dynamics, there is a need for quantitative metrics to interpret wastewater data in the context of public health trends. 24-hour composite wastewater samples were collected from March 2020 through May 2021 from a Massachusetts wastewater treatment plant and SARS-CoV-2 RNA concentrations were measured using RT-qPCR. The relationship between wastewater copy numbers of SARS-CoV-2 gene fragments and COVID-19 clinical cases and deaths varies over time. We demonstrate the utility of three new metrics to monitor changes in COVID-19 epidemiology: (1) the ratio between wastewater copy numbers of SARS-CoV-2 gene fragments and clinical cases (WC ratio), (2) the time lag between wastewater and clinical reporting, and (3) a transfer function between the wastewater and clinical case curves. The WC ratio increases after key events, providing insight into the balance between disease spread and public health response. Time lag and transfer function analysis showed that wastewater data preceded clinically reported cases in the first wave of the pandemic but did not serve as a leading indicator in the second wave, likely due to increased testing capacity, which allows for more timely case detection and reporting. These three metrics could help further integrate wastewater surveillance into the public health response to the COVID-19 pandemic and future pandemics.
Keywords	COVID-19 infection ; RNA ; Severe acute respiratory syndrome coronavirus 2 ; genes ; monitoring ; pandemic ; public health ; research ; wastewater ; wastewater treatment ; water ; Massachusetts
Language	English
Dates of publication	2022-0401
Publishing place	Elsevier Ltd
Document type	Article
ZDB-ID	202613-2
ISSN	1879-2448 ; 0043-1354
ISSN (online)	1879-2448
ISSN	0043-1354
DOI	10.1016/j.watres.2022.118070
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Article ; Online: Nationwide Trends in COVID-19 Cases and SARS-CoV-2 RNA Wastewater Concentrations in the United States.

ACS ES&T water

2022 Volume 2, Issue 11, Page(s) 1899–1909

Abstract: Wastewater-based epidemiology has emerged as a promising technology for population-level surveillance of COVID-19. In this study, we present results of a large nationwide SARS-CoV-2 wastewater monitoring system in the United States. We profile 55 ... ...

Abstract	Wastewater-based epidemiology has emerged as a promising technology for population-level surveillance of COVID-19. In this study, we present results of a large nationwide SARS-CoV-2 wastewater monitoring system in the United States. We profile 55 locations with at least six months of sampling from April 2020 to May 2021. These locations represent more than 12 million individuals across 19 states. Samples were collected approximately weekly by wastewater treatment utilities as part of a regular wastewater surveillance service and analyzed for SARS-CoV-2 RNA concentrations. SARS-CoV-2 RNA concentrations were normalized to pepper mild mottle virus, an indicator of fecal matter in wastewater. We show that wastewater data reflect temporal and geographic trends in clinical COVID-19 cases and investigate the impact of normalization on correlations with case data within and across locations. We also provide key lessons learned from our broad-scale implementation of wastewater-based epidemiology, which can be used to inform wastewater-based epidemiology approaches for future emerging diseases. This work demonstrates that wastewater surveillance is a feasible approach for nationwide population-level monitoring of COVID-19 disease. With an evolving epidemic and effective vaccines against SARS-CoV-2, wastewater-based epidemiology can serve as a passive surveillance approach for detecting changing dynamics or resurgences of the virus.
Language	English
Publishing date	2022-05-03
Publishing country	United States
Document type	Journal Article
ISSN	2690-0637
ISSN (online)	2690-0637
DOI	10.1021/acsestwater.1c00434
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Article ; Online: Metrics to relate COVID-19 wastewater data to clinical testing dynamics.

Water research

2022 Volume 212, Page(s) 118070

Abstract	Wastewater surveillance has emerged as a useful tool in the public health response to the COVID-19 pandemic. While wastewater surveillance has been applied at various scales to monitor population-level COVID-19 dynamics, there is a need for quantitative metrics to interpret wastewater data in the context of public health trends. 24-hour composite wastewater samples were collected from March 2020 through May 2021 from a Massachusetts wastewater treatment plant and SARS-CoV-2 RNA concentrations were measured using RT-qPCR. The relationship between wastewater copy numbers of SARS-CoV-2 gene fragments and COVID-19 clinical cases and deaths varies over time. We demonstrate the utility of three new metrics to monitor changes in COVID-19 epidemiology: (1) the ratio between wastewater copy numbers of SARS-CoV-2 gene fragments and clinical cases (WC ratio), (2) the time lag between wastewater and clinical reporting, and (3) a transfer function between the wastewater and clinical case curves. The WC ratio increases after key events, providing insight into the balance between disease spread and public health response. Time lag and transfer function analysis showed that wastewater data preceded clinically reported cases in the first wave of the pandemic but did not serve as a leading indicator in the second wave, likely due to increased testing capacity, which allows for more timely case detection and reporting. These three metrics could help further integrate wastewater surveillance into the public health response to the COVID-19 pandemic and future pandemics.
MeSH term(s)	Benchmarking ; COVID-19 ; Humans ; Pandemics ; RNA, Viral ; SARS-CoV-2 ; Wastewater ; Wastewater-Based Epidemiological Monitoring
Chemical Substances	RNA, Viral ; Waste Water
Language	English
Publishing date	2022-01-14
Publishing country	England
Document type	Journal Article
ZDB-ID	202613-2
ISSN	1879-2448 ; 0043-1354
ISSN (online)	1879-2448
ISSN	0043-1354
DOI	10.1016/j.watres.2022.118070
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