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Open-File Report 2010–1102

Prepared in cooperation with the
New York State Department of Environmental Conservation

Method Description, Quality Assurance, Environmental Data, and other Information for Analysis of Pharmaceuticals in Wastewater-Treatment-Plant Effluents, Streamwater, and Reservoirs, 2004-2009

By Patrick J. Phillips, Steven G. Smith, Dana W. Kolpin, Steven D. Zaugg, Herbert T. Buxton, and Edward T. Furlong

ABSTRACT

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Wastewater-treatment-plant (WWTP) effluents are a demonstrated source of pharmaceuticals to the environment. During 2004-09, a study was conducted to identify pharmaceutical compounds in effluents from WWTPs (including two that receive substantial discharges from pharmaceutical formulation facilities), streamwater, and reservoirs. The methods used to determine and quantify concentrations of seven pharmaceuticals are described. In addition, the report includes information on pharmaceuticals formulated or potentially formulated at the two pharmaceutical formulation facilities that provide substantial discharge to two of the WWTPs, and potential limitations to these data are discussed. The analytical methods used to provide data on the seven pharmaceuticals (including opioids, muscle relaxants, and other pharmaceuticals) in filtered water samples also are described. Data are provided on method performance, including spike data, method detection limit results, and an estimation of precision. Quality-assurance data for sample collection and handling are included. Quantitative data are presented for the seven pharmaceuticals in water samples collected at WWTP discharge points, from streams, and at reservoirs. Occurrence data also are provided for 19 pharmaceuticals that were qualitatively identified. Flow data at selected WWTP and streams are presented.

Between 2004-09, 35-38 effluent samples were collected from each of three WWTPs in New York and analyzed for seven pharmaceuticals. Two WWTPs (NY2 and NY3) receive substantial inflows (greater than 20 percent of plant flow) from pharmaceutical formulation facilities (PFF) and one (NY1) receives no PFF flow. Samples of effluents from 23 WWTPs across the United States were analyzed once for these pharmaceuticals as part of a national survey. Maximum pharmaceutical effluent concentrations for the national survey and NY1 effluent samples were generally less than 1 µg/L. Four pharmaceuticals (methadone, oxycodone, butalbital and metaxalone) in samples of NY3 effluent had median concentrations ranging from 3.4 to greater than 400 µg/L. Maximum concentrations of oxycodone (1,700 µg/L) and metaxalone (3,800 µg/L) in samples from NY3 effluent exceeded 1,000 µg/L. Three pharmaceuticals (butalbital, carisoprodol, and oxycodone) in samples of NY2 effluent had median concentrations ranging from 2 to 11 µg/L. These findings suggest that current manufacturing practices at these PFFs can result in pharmaceutical concentrations from 10 to 1,000 times higher than those typically found in WWTP effluents.

First posted June 3, 2010

For additional information contact:
Director
U.S. Geological Survey
New York Water Science Center
425 Jordan Road
Troy, NY 12180-8349
(603)226-7800

http://ny.water.usgs.gov

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Suggested citation:

Phillips, P.J., Smith, S.G., Kolpin, D.W., Zaugg, S.D., Buxton, H.T., and Furlong, E.T., 2010, Method Description, Quality Assurance, Environmental Data, and other Information for Analysis of Pharmaceuticals in Wastewater-Treatment-Plant Effluents, Streamwater, and Reservoirs, 2004-2009: U.S. Geological Survey Open-File Report 2010-1102, 36 p., (Also available at https://pubs.usgs.gov/of/2010/1102/.)



Contents

Abstract

Introduction

Purpose and Scope

Sampling Network

Information on Pharmaceuticals Formulated at PFFs

Method Description

Sample Preparation, Apparatus, Instrumentation, and Standards

Qualitative and Tentative Identification of Analytes

Quantitation of Analytes

Quantifying High Concentrations

Quantifying Low Concentrations

Method Performance

Spike

Reagent Set Spike2

Matrix Spikes

NY3 Effluent Matrix Spikes

NY1 Effluent Matrix Spikes

NY4 Effluent Matrix Spikes

NY1 Upstream Matrix Spikes

Summary of Reagent Set and Matrix Spikes

Method Detection Limit

Estimation of Precision

Holding Time Study

Environmental Data

Quality-Assurance Data

Blank Data

Replicate Data

Environmental Data for Pharmaceuticals in Wastewater-Treatment Plants, and in Streamwater and Reservoir Water

Concentrations in Samples from National Survey of Wastewater-Treatment-Plant Effluent

Concentrations in Effluent Samples from Wastewater-Treatment Plants NY1, NY2 and NY3.

Concentrations in Samples of Streamwater Collected Downstream from WWTP Discharge Points of NY1, NY2, and NY3

Concentrations in Samples of Streamwater Collected Upstream from WWTP NY1, NY2, and NY3 Discharge Points

Concentrations in Samples collected from Reservoirs and Additional Streams Downstream from NY2 Effluent Discharge Point

Data on Qualitatively and Tentatively Identified Compounds

Flow Data for Selected WWTP Effluent Samples and Streamwater Samples

Summary

Acknowledgments

References Cited



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