Occurrence of Antibiotic Compounds in Source Water and

U.S. Department of the InteriorU.S. Geological Survey

Scientific Investigations Report 2010–5083

In cooperation with the City of Columbus, Ohio

Occurrence of Antibiotic Compounds in Source Water and Finished Drinking Water from the Upper Scioto River Basin, Ohio, 2005–6


By Dennis P. Finnegan, Laura A. Simonson, and Michael T. Meyer

In cooperation with the City of Columbus, Ohio

Scientific Investigations Report 2010–5083

U.S. Department of the InteriorU.S. Geological Survey

U.S. Department of the InteriorKEN SALAZAR, Secretary

U.S. Geological SurveyMarcia K. McNutt, Director

U.S. Geological Survey, Reston, Virginia: 2010

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Suggested citation:Finnegan, D.P., Simonson, L.A., and Meyer, M.T., 2010, Occurrence of antibiotic compounds in source water and fin-ished drinking water from the upper Scioto River Basin, Ohio, 2005–6: U.S. Geological Survey Scientific Investigations Report 2010–5083, 16 p. plus appendixes.

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iii

Contents

Acknowledgments ........................................................................................................................................viAbstract ...........................................................................................................................................................1Introduction.....................................................................................................................................................1

Purpose and Scope ..............................................................................................................................2Previous Studies ...................................................................................................................................3Description of Study Area ...................................................................................................................5

Methods...........................................................................................................................................................5Field Methods ........................................................................................................................................5Quality-Control Procedures ................................................................................................................8Sample Analysis ....................................................................................................................................8

Occurrence of Antibiotics ............................................................................................................................9Summary and Conclusions .........................................................................................................................15References Cited..........................................................................................................................................15Appendix 1. Water-Quality Analyses and Quality-Control Results...................................................18Appendix 2. Sample Analysis .................................................................................................................38

Figures 1. Graph showing detection frequencies for selected antibiotics. A, The upper

Scioto River Basin study, 2005–6. B, The National Reconnasiance,1999–2000 .................4 2–3 Maps showing: 2.. Land use in and around study area, upper Scioto River Basin,

central Ohio ..........................................................................................................................6 3. Sampling locations, upper Scioto River Basin, Ohio, 2005–6 .......................................7 4–8. Graphs showing: 4. Occurrence and concentrations of antibiotic compounds at sites in the

upper Scioto River Basin, Ohio, and corresponding detection frequencies evaluated against each compound’s miminum reporting level .................................11

5. Total number of detections (61) by antibiotic group for collection sites in the upper Scioto River Basin, 2005–6 ............................................................................12

6. Summary of antibiotic compounds detected in water samples collected from the upper Scioto River Basin, Ohio, 2005–6 .........................................................12

7. Numbers of detections of antibiotic compounds by sampling site and date in source and finished waters of the upper Scioto River Basin, central Ohio, 2005–6 ..........................................................................................................13

8. Total number of detections at all sites, by season, in the upper Scioto River Basin, central Ohio, 2005–6 ............................................................14

iv

Tables 1. Major antibiotic groups and some common uses in human therapy and

animal husbandry .........................................................................................................................2 2. Major groups of antibiotics and degradation products targeted by

chemical analysis of water samples collected from the upper Scioto River Basin, Ohio, 2005-6 .....................................................................................3

3. Sampling-locations descriptions for antibiotic samples collected in the upper Scioto River Basin, Ohio, 2005–6 ....................................................................................8

4. Total numbers of detections of antibiotic compounds in source- and finishedwater sites from the Scioto River Basin, Ohio, 2005–6 ........................................10

Appendix Tables 1–1. Field parameters from sampling locations in the

upper Scioto River Basin, Ohio, 2005–6 ........................................................................... 18–19 1–2. Water-quality analyses from sampling locations in the

upper Scioto River Basin, Ohio, 2005–6 ........................................................................... 20–33 1–3. Quality-control analyses from sampling locations in the

upper Scioto River Basin, Ohio, 2005–6 ........................................................................... 34–37 2–1. Mobile phases used in the liquid chromatography/electrospray

ionization-mass spectrometry (LC/ESI-MS) techniques for three common antibiotic groups ..............................................................................................38

v

Conversion Factors and Abbreviations

Multiply By To obtain

Length

millimeter(mm) 0.03937 inch(in.)

mile(mi) 1.609 kilometer(km)

Area

squaremile(mi2) 259.0 hectare(ha)

squaremile(mi2) 2.590 squarekilometer(km2)

Volume

milliliter(mL) .03381 fluidounce(oz)

microliter(µL) .001 milliliter

liter(L) .2642 gallon(gal)

Flow rate

cubicfootpersecond(ft3/s) .02832 cubicmeterpersecond(m3/s)

Temperature in degrees Celsius (°C) may be converted to degrees Fahrenheit (°F) as follows: °F=(1.8×°C)+32

Specific conductance is given in microsiemens per centimeter at 25 degrees Celsius (µS/cm at 25 °C).

Concentrations of chemical constituents in water are given in milligrams per liter (mg/L), micrograms per liter (µg/L), or nanograms per milliliter (ng/mL).

Pore sizes of filters are given in micrometers (µm; a micrometer is 0.001 millimeter).

vi

Acknowledgments

The authors thank Matt Steele and Rod Dunn from the City of Columbus, Division of Power and Water, for their assistance in project planning and report review


By Dennis P. Finnegan, Laura A. Simonson, and Michael T. Meyer

Abstract

Theoccurrenceofantibioticsinsurfacewaterandgroundwaterinurbanbasinshasbecomeatopicofincreas-inginterestinrecentyears.Littleisknownabouttheoccur-rence,fate,ortransportofthesecompoundsandthepossiblehealtheffectsinhumansandaquaticlife.TheU.S.GeologicalSurvey,incooperationwiththeCityofColumbus,DivisionofPowerandWater,didastudytoprovideasynopticviewoftheoccurrenceofantibioticsinsourceandfinishedwatersintheupperSciotoRiverBasin.

Watersampleswerecollectedseasonally—winter(December2005),spring(May2006),summer(August2006)andfall(October2006)—atfivesurface-watersites,onegroundwatersite,andthreewater-treatmentplants(WTPs).WithintheupperSciotoRiverBasin,samplingateachWTPinvolvedtwosamplingsites:asource-waterintakesiteandafinished-watersite.

Oneormoreantibioticsweredetectedat11ofthe12samplingsites.Ofthe49targetedantibioticcompounds,12(24percent)weredetectedatleastonetimeforatotalof61detectionsoverall.Thesecompoundswereazithromycin,tylosin,erythromycin-H2O,erythromycin,roxithromycin,ciprofloxacin,ofloxacin,sulfamethazine,sulfamethoxazole,iso-chlorotetracycline,lincomycin,andtrimethoprim.Detec-tionresultswereatlowlevels,withanoverallmedianof0.014µg/L.HapCremeanWTPhadthefewestdetections,withtwosource-waterdetectionsofsulfamethoxazoleandazithromycinandnodetectionsinthefinishedwater.Ofthetotalof61detections,31wereinthewintersamplerun.Sulfamethoxazaleandazithromycindetectionsrepresent41percentofallantibioticdetections.Azithromycinwasdetectedonlyinthewintersample.Someantibiotics,suchasthoseinthequinolineandtetracyclinefamilies,dissipatemorequicklyinwarmwater,whichmayexplainwhytheyweredetectedinthecoolmonths(winter,spring,andfall)andnotinthesummer.Antibioticdatacollectedduringthisstudywerecomparedtoantibioticdatacollectedinpreviousnational,regional,andlocalstudies.ManyofthesameantibioticcompoundsdetectedintheupperSciotoRiverBasinalsoweredetectedinthoseinvestigations.

Introduction

Anationalreconnaissancestudydoneduring1999–2000revealedthatavarietyofchemicalsuseddailyinhomes,industry,andagriculture and includingantimicrobials,deter-gents,disinfectants,fragrances,fireretardants,prescriptionandnonprescriptiondrugs,andpesticides can enter streams (Kolpin and others, 2002). These chemicals, which can also affect groundwater, are often referred to as emerging contami-nants (ECs), organic wastewater compounds (OWCs), and pharmaceuticals and personal care products (PPCPs); they can be released into the environment by various discharges (indus-trial facilities, animal feedlots, wastewater-treatment plants, septic disposal systems) and land applications (sludge, biosol-ids, or animal waste) in urban or agricultural areas. AntibioticsareconsideredtobeECsandcannowbedetectedatlowcon-centrationsinsurfacewaterandgroundwater(U.S.GeologicalSurvey,2007). A recent study in Ohio detected antibiotics at low concentrations (parts per billion) in streams draining the Great and Little Miami River Basins (Rowe and others, 2004).

Thepotentialeffectsonhumansandbiotaresultingfromenvironmentalexposuretoantibioticsarenotwellunderstood,but ongoing research indicates possible chronic effects from long-term exposure to even trace concentrations (Kolpin and others, 2002). Largequantitiesofantibioticsareadministeredeveryyeartohumansandanimalstopreventandtreatdiseasesandinfection(table1).Forsomeconfinedlivestock,antibioticsareusedtopromotegrowth(Huangandothers,2001). Little is known about the effects of many other individual chemicals or about the potential additive or synergistic effects of mixtures of these chemicals. Asmuchas90percentofsomeadministeredantibioticscanbeexcretedwithoutundergoingmetabolism,whichmakesthemavail-ableto bioaccumulate or biomagnify in aquatic or terrestrial organisms (Halling-Sørensen and others, 1998). Few studies have addressed the occurrence, fate, or transport of antibiotic compounds in the environment, and water-quality standards to protect human or aquatic health have not been established for most of these chemicals.

2 Antibiotic Compounds in Source Water and Finished Drinking Water, Upper Scioto River Basin, Ohio, 2005–6

Intherecentpast,analyticalmethodswerenotavailabletoaccuratelydetectextremelylowconcentrationsofantibioticcompoundsinwaterandprovideabasisfordrinking-waterstandards.Analyticalmethodshavenowbeenimprovedtoincludeabroaderrangeofantibioticcompoundsforanalysis,aswellastheabilitytoreportdetectionsinconcentrationsaslowaspartsperbillion(ppb).Developmentofdrinking-waterstandardsgenerallyinvolveslong-termexposurestudiesofknownhealtheffects;asaresult,noMaximumContaminantLevels(MCLs),HealthAdvisoryLevels(HALs),orHealth-BasedScreeningLevels(HBSLs)formostofthesecom-poundshaveyetbeenestablished(Kolpinandothers,2002).

Although human health and environmental effects of antibiotics are not well understood, other chemicals—such as the antimicrobial compound triclosan found in many liquid soaps, dishwasher powders, and plastics—are suspected of increasing antibiotic resistance in bacteria in the environment, and similar concerns have been raised by large-scale use of veterinary antibiotics in confined animal feeding operations (Kolpin and others, 2002).

As a result of attention on the issue of antibiotics in public water supplies (Stratton, 2002), the City of Columbus, Ohio, received inquiries regarding the presence of antibiotics, and other wastewater chemicals in city water supplies. Con-sequently, the U.S. Geological Survey (USGS), in coopera-tion with the City of Columbus, collected water samples from

locations in the upper Scioto River Basin from December 2005 to October 2006 to determine the occurrence and distri-bution of antibiotic compounds in source water from the City of Columbus, Ohio, during different hydrologic conditions. Sampleswerecollectedfromfivesurface-watersites,onegroundwatersite,andtwosites—asourceandfinishedwatersite—ateachofthreewater-treatmentplants(WTPs).Sampleswereanalyzedfor49antibioticcompounds,whichwere grouped into five classes: macrolides, beta lactams, quino-lines, sulfonamides, and tetracyclines (table 2). A sixth group analyzed for, “other antibiotics,” included compounds such as carbadox and lincomycin (table 2).

Purpose and Scope

Thepurposeofthisreportistopresentanddescribedatafromthe2005–6study.Resultsfromthisstudyaddressdatagapsfromapreviousreconnaissanceeffortin2001(see“PreviousStudies”section;Kolpinandothers,2002)andcomplementongoingeffortsbytheUSGSToxicSub-stancesHydrologyProgramandtheUSGSNationalWater-QualityAssessmentProgramtocharacterizethedistributionandoccurrenceofantibioticsandOWCsintheNation’swaterresources.

Table 1. Major antibiotic groups and some common uses in human therapy and animal husbandry.

[Sources:Hooper,D.C.,1998;Smilack,J.D.,1999;Čižmanandothers,2001;Huangandothers,2001;Lipsitchandothers,2002;Casewellandothers,2003;andScholar,E.M.,2003]

Antibiotic group

Tetracyclines Sulfonamides and quinolones Macrolides and beta lactams

Human-therapy treatment types

Atypicalpneumoniasyndromes Urinary-tractinfections

Respiratoryinfections

Community-acquiredpneumonia

ChlamydialinfectionsRespiratoryinfections

Community-acquiredpneumonia Strepthroat

Rickettsialinfections

RockyMountainspottedfever Chronicbronchitis Laryngitis

Typhus Gastrointestinalinfections

Gastroenteritis Sinusitis

Qfever Diarrhea Meningitis

Lymedisease Boneandskininfections

Osteomyelitis

Skininfections

Impetigo

Ehrlichiosis Staphinfections Erysipelas

Acne Venerealdiseases

Chlamydialinfections

Cellulitis

Rosacea Middle-earinfections

Animal-husbandry treatment types

GrowthpromotionBacterialinfections

GrowthpromotionDiseaseprevention

Introduction 3

Previous Studies

InvestigationsintotheoccurrenceofECsinsurfacewatershavebeendoneatnational,regional,andlocallevelsnationwide,andresultsindicatethatantibioticcompoundsarenotuncommoningroundwaterandsurfacewater.In2002,USGSreportedonthefirstnationalreconnaissanceoftheoccurrenceofpharmaceuticals,hormones,andotherOWCsinwaterresources(Kolpinandothers,2002).Anetworkof139streamsacross30stateswassampledandanalyzedfor95ECs.Somecommonlydetectedantibioticsreportedinthatstudywerelincomycin(19.2percentdetection)andtylosin(13.5percentdetection;fig.1).Oftheantibioticssampledfor,45percentweredetected,thehighestfrequencybeingforerythromycin-H2Oatroughly21.5percent.Mostdetectionswereatlowconcentrations;however,chroniceffectsfromlow-levelenvironmentalexposurehavepotentialtopromoteantibioticresistance(Kolpinandothers,2002).

Attheregionallevel,briefinvestigationsintoECsintheStillwaterRiverBasinandtheGreatMiamiRiverBasinwerecompletedin2000.ThirtysamplescollectedfromsubbasinsintheStillwaterRiverBasinafterasinglehigh-floweventrevealedmultiplelincomycindetectionsandanerythromycin-H2Odetectionincombinationwithlincomycin.Lincomycin(23.5percent)wasfoundatsimilarfrequenciesinthisregionalstudy(Roweandothers,2004)andthenationalinvestigation(Kolpinandothers,2002).Traceamountsofsulfamethazineandsulfadimethoxinealsoweredetectedinspringrunoffsam-plesintheStillwaterRiverBasin(Roweandothers,2004).

In2001,theUSGSperformedasmall-scalelocalrecon-naissancestudywithinthecurrentstudyunitboundariestoevaluatethepresenceofantibioticsinsourcewaterandfinisheddrinkingwatersuppliedbytheCityofColumbus.Onetothreesampleswerecollectedatthreesurface-watersites(PowderLickRunnearSummersville,Ohio;MillCreekbelowMarysville,Ohio;andSciotoRivernearProspect,Ohio)intheSciotoRiverBasinupstreamfromthesource-waterintaketotheDublinRoadWTP.Inaddition,source-andfinished-watersampleswerecollectedattheDublinRoadandHapCremeanWTPs.Noantibioticsweredetectedatanyofthethreesurface-watersites.However,threeantibioticcompoundsweredetectedinonesampleevent(Dec.5,2001)attheDublinRoadWTP:lincomycin(0.03µg/L)andsulfadi-methoxine(0.01µg/L)weredetectedinthesourcewater,andvirginiamycin(0.15µg/L)wasdetectedinthefinishedwater(USGSOhioWaterScienceCenter,unpub.data,2001).

Table 2. Major groups of antibiotics and degradation products targeted by chemical analysis of water samples collected from the upper Scioto River Basin, Ohio, 2005-6.

Macrolides and degradation products

Tetracyclines and degradation products

Azithromycin Chlorotetracycline

Erythromycin Anhydro-Chlorotetracycline

Erythromycin-H20 Epi-anhydro-Chlorotetracycline

Roxithromycin Epi-chlorotetracycline

Tylosin Epi-iso-chlorotetracycline

Virginiamycin Iso-chlorotetracycline

Demeclocycline

Beta Lactams Doxycycline

Amoxicillin Minocycline

Ampicillin Oxytetracycline

Cefotaxime Alphaapo-oxytetracycline

Cloxacillin Betaapo-oxytetracycline

Oxacillin Epi-oxytetracycline

PenicillinG Tetracycline

PenicllinV Anhydro-tetracycline

Epi-anhydro-tetracycline

Quinolines Epi-tetracycline

Ciprofloxacin

Clinafloxacin Other antibiotics

Flumequine Carbadox

Lomefloxacin Lincomycin

Norfloxacin Ormetoprim

Ofloxacin Trimethoprim

OxolinicAcid

Sarafloxacin

Sulfonamides

Sulfachlorpyradazine

Sulfadiazine

Sulfadimethoxine

Sulfamerazine

Sulfamethazine

Sulfamethoxazole

Sulfathiazole

SCIOTO RIVER BASIN STUDY2005–6

39 samples

NATIONAL RECONNAISSANCE1999–2000

104 samplesA B

Trimethroprim

Linomycin

Iso-Chlorotetracyline

Sulfamethoxazole

Sulfamethazine

O�oxacin

Cipro�oxacin

Roxithromycin

Erythromycin

Erythromycin-H20

Tylosin

Azithromycin

DETECTION FREQUENCY, IN PERCENT

0 10 20 30 40 50 0 10 20 30 40 50

NS

NS

NS

NS


Figure 1. Detection frequencies for selected antibiotics. A, The upper Scioto River Basin study, 2005–6. B, The National Reconnasiance,1999–2000 (Kolpin and others, 2002). (NS, not sampled for.)

Methods 5

Description of Study Area

TheupperSciotoRiverBasindrainsapproximately2,300mi2ofcentralandnorth-centralOhio,stretchingfromCrawfordCountyatthenorthernmostpointtoFranklinCountyatthesouth(fig.2).TheSciotoisthelongestfree-flowingriverinOhioat231milong,anditisfedby3,000milesoftributariesthatflowthroughcentralandnorth-centralOhio(NatureConservancy,2007;ResourcesFirstFoundation,2007).ThesurficialgeologyoftheSciotoRiverBasinconsistsofglacialandalluvialdeposits(Oblingerandothers,1991).TheSciotoRiverBasinisalargelyagriculturalareathatincludesnumeroussuburbancommunitiesnorthofColumbus(fig.2).Drainagefromagricultural,residential,municipal,andindustrialactivitiesinthebasinresultsinrunoffofnutrients,pesticides,andavarietyofECstosurfacewater(Roweandothers,2004).Thebasinalsocontainsconfinedanimalfeed-ingoperations(CAFOs)andnumerouswastewater-treatmentplantsthatdischargeintotheSciotoRiver(fig.2).Thebasinhasapopulationofapproximately2millionpeopleandisamajorsourceofpublicdrinkingwater;morethan20municipalwatersystemsdrawsurfacewaterandgroundwaterfromtheSciotoRiver,itstributaries,orwellsadjacenttoitstributaries(ResourcesFirstFoundation,2007).TheCityofColumbusdraws85percentofthecity’sannualwatersupply(roughly47.5billiongallonsofwater)fromthreereservoirsintheSciotoRiverBasin—Griggs,O’Shaughnessy,andHoover—whichhaveacombinedstoragecapacityofabout27billiongallons(Columbus DepartmentofPublicUtilities, 2009).

Methods

Field Methods

FromDecember2005throughOctober2006(wateryears2006and2007),USGSpersonnelcollectedwatersamplestobeanalyzedforantibioticsat12selectedsamplingsites.Sampleswerecollectedonaquarterlyschedule,inanattempttocaptureidealhydrologicconditionswithineachseason.Fieldblanksandreplicateswerescheduledtobesampledinassociationwitheachenvironmentalquarterlysample.

Surface-watersampleswerecollectedfromfarthestupstreamtodownstreamandfromwesttoeastbyusingadepth-andwidth-integrated,equal-width-increment(EWI)method(Wildeandothers,2006).Twomodelsofisokineticsamplersincorporatingal-LTeflonbottlewereusedforsurface-watercollection:aDH-95wasusedfromabridge,andaDH-81wasusedforwading.ThecollectedsamplewascompositedintoaTeflonchurnsplittertoobtainahomoge-neoussubsample(Wildeandothers,2006).Thesurface-watersiteswere(1)PowderLickRunnearSummersville,Ohio,(2)MillCreekbelowMarysville,Ohio,(3)BigWalnutCreekatSunbury,Ohio,(4)SciotoRivernearProspect,Ohio,and(5)SciotoRiverdownstreamfromCollectorWell-104

(CW-104)(fig.3,table3).Groundwatersampleswerecol-lectedfromsite(6)ColumbusWellFieldCollectorWell-101(CW-101)—intheColumbusSouthwellfield—whichsuppliesgroundwatertotheParsonsAvenueWTP.Thissitewassampledbymeansofthegrab-samplemethodfromaconstantlyflowingspigotwithinthewellhouse.Pairedsource-andfinished-drinking-watergrabsampleswerecollectedattheDublinRoadPlant(7,8),theHapCremeanPlant(9,10),andtheParsonsAvenuePlant(11,12)(fig.3;table3).

Allsampleswereprocessedatthetimeofcollection.Samplewaterwasfilteredthrougha0.7-µmbakedglass-fiberfilterandcapturedintwo125-mL,bakedamber-glassbottles(Wildeandothers,2004).SampleswerechilledandshippedovernighttotheUSGSOrganicGeochemistryResearchGroupLaboratory(ORGL)inLawrence,Kansas.Ancillarydatacol-lectedateachsiteincludedtemperature,pH,specificcon-ductance,anddissolvedoxygenconcentrations(appendix1,table1–1).Streamflowwasmeasuredatungagedstreamsites1and2(fig.3;table3). Each sampling event required 1 week for collection and processing of samples from all 12 sites.

Becauseofsomewhatatypicalweatherpatterns,samplecollectionconsistedoflow-flowsamplesinDecember2005andAugust2006,andrunoffsamplesinMay2006andOcto-ber2006.Also,becauselargeCAFOsarepresentintheupperSciotoRiverBasin,anadditionalrunoffsamplewascollectedinAugustatthestreamsitesintheupperScioto—PowderLickRunnearSummersville,MillCreekbelowMarysville,SciotoRivernearProspect,andtheDublinRoadWTPsites—tofacilitateassessmentofrunoffwaterquality.Theremainingsites—BigWalnutCreekatSunbury,theColumbusWellFieldCW-101,SciotoRiverdownstreamfromCW-104,andHapCremeanandParsonsWTPs—weresampledonce(May)dur-ingrunoffconditions.

SeasonalrunoffsampleswerescheduledforcollectioninMay–June(tocapturehighflowsearlyinthegrowingseason)andJuly–August(tocapturelowflowslaterinthegrowingseason).However,moreimportancewasgiventocollect-ingatleastonesetofsamplesduringeachseasonalquarterthantosamplingthetypesofhydrologicaleventsexpectedduringthosequarters.Atypicalweatherconditionsresultedinsamplesbeingcollectedearlierorlaterthanexpected,wheneversuitablelow-floworrunoffconditionspresentedthemselves.Streamrunoffsampleswerecollectedduringorimmediatelyaftersignificantrainfall.Nothresholdrainfallamountwasdefinedforatriggeredsamplingrun;seasonaltiming,morethananything,withsufficientrainfallusuallydictatedwhentosample.Source-waterandfinished-drinking-watersampleswerecollected3–5dayslater.Inanefforttotargetworst-caseconditions,sampleswerecollectedduringperiodswhenresultsofdailynitrateandpesticidemonitoringdonebytheColumbusDivisionofPowerandWaterindicatedthatconcentrationsofagrochemicalswerehighestinthesourcewater.Low-flowsampleswerecollectedinlatesum-merinanefforttotargetperiodswhentreatedwastewaterandseptic-tankdischargelikelyrepresentalargerproportionofthetotalstreamflow.

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Landcover data from U.S. Geological Survey, 2001National Land Cover Datasetprojection, Albers; North American Datum of 1983.

Figure 2. Land cover in and around study area, Upper Scioto River Basin, Ohio.

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0 10 20 MILES

0 10 20 KILOMETERS

EXPLANATION

#* Wastewater-treatement plant

_̀ Confined animal feeding operations

Study area boundary

Open water

Developed, open space and low intensity

Developed, medium and high intensity

Forest

Agriculture

Other

Alum CreekReservoir


Figure 2. Land use in and around study area, upper Scioto River Basin, central Ohio.

Figure 3. Sampling locations, Upper Scioto River Basin, Ohio, 2005–6. (Numbers refer to site descriptions listed in table 3.)

Base from Ohio Department of Natural Resources, Division of Real Estate and Land Management,1999; scale 1:24,000; State Plane South; North American Datum of 1927.

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EXPLANATION

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Methods 7

Figure 3. Sampling locations, upper Scioto River Basin, Ohio, 2005–6. (Numbers refer to site descriptions listed in table 3.)


Quality-Control Procedures

Thequality-control(QC)procedures,whichconsistedofcollectingandanalyzingfieldblanksandreplicates,followedageneralquality-assurance/qualitycontrolprotocolestab-lishedforlow-levelorganicanalyses(partsperbillion),thesameprotocolusedforpesticidesintheNAWQAProgram(Muellerandothers,1997).Becausemanyofthecompoundsbeingsampledforwerecommonlyusedproducts(personalcareproductsandmedicines,forexample)andtheriskforaccidentalcontaminationwashigh,arelativelylargenum-beroffieldblankswerecollectedcomparedtotheNAWQApesticideprotocolfortheprojecttoidentifyandresolvepossiblecontaminationissues.Antibioticfield-blanksamplesrepresentedabout15percentoftheenvironmentalsamplesandyieldednodetections.Replicatesweresamplesthatwerecollectedinanidenticalmannerasenvironmentalsamplesasameasureofvariabilityofthecollectionandanalysisprocess.TworeplicatesampleswerecollectedatstudysitesColumbusWellFieldCW-101andPowderLickRunnearSummersville,Ohio.Thereplicatesindicatedgoodreproducibilityoflabora-toryresultswithanidenticalconcentrationof(0.005µg/L)forlincomycin,theonlydetectionfromthetworeplicatesamples.Fieldspikes—samplesaugmentedwithknownquantitiesandconcentrationsofanalytesorsurrogatesandoftenusedasa

QCcheckinwater-qualitystudies—werenotcollectedduringthisinvestigationbecausetherewerenoavailablefieldspikesurrogatesatthetimeofthisinvestigation.AllQCresultsforthestudyarelistedinappendix1,table1–3.

Sample Analysis

SampleswereanalyzedattheORGLinLawrence,Kansas,forfiveclassesofantibiotics—betalactams,macro-lides,quinolones,sulfonamides,andtetracyclines—byuseofthreeonlinesolid-phaseextraction(SPE)methodsandliquidchromatography/massspectrometry(LC/MS)orLC/MS/MS.Thisapproachcancurrentlydetermine49commonlyusedhuman-therapyandanimal-husbandryantibiotics,includingsomeantibioticbreakdownproductsordegradates(tables1and2).Betalactamsandmacrolides(BLM),sulfonamidesandquinolones(SQ),andthetetracyclines(TET)wereanalyzedseparatelybyuseofonlinesolidSPEmethodsandliquidchromatography/electrosprayionization-massspectrometry(LC/ESI-MS)inpositive-ionmode.Thereportinglevelsrangedfrom0.01to0.005µg/L.(Seeappendix2foramoredetaileddescriptionofBLM,SQ,andTETsampleanalysis;Meyerandothers,2007.)

Table 3. Sampling-locations descriptions for antibiotic samples collected in the upper Scioto River Basin, Ohio, 2005–6.

[WTP,water-treatmentplant;DS,downstream;CW,collectorwell;I,waterintake;F,finishedwater]

Map identification number (location shown

in fig. 1)

Station identification number

Station name Relation to water-treatment plants

1 402302083254100 PowderLickRunnearSummersville UpstreamfromtwoWTPs.

2 401425083212500 MillCreekbelowMarysville UpstreamfromtwoWTPs.

3 03228300 BigWalnutCreekatSunbury UpstreamfromtwoWTPs.

4 03219500 SciotoRivernearProspect UpstreamfromtwoWTPs.

5 395033083002900 SciotoRiverDSfromCW-104 DownstreamfromoneWTP.

6 395111083010600 ColumbusWellFieldCW-101 AdjacenttooneWTP;wellsample.

7` 395813083020701 DublinRoadWTP,I AtWTP.

8 395813083020702 DublinRoadWTP,F AtWTP.

9 400336082533901 HapCremeanWTPI AtWTP.

10 400336082533902 HapCremeanWTP,F AtWTP.

11 395050082591301 ParsonsAvenueWTP,I AtWTP.

12 395050082591302 ParsonsAvenueWTP,F AtWTP.

Occurrence of Antibiotics 9

Occurrence of Antibiotics

Antibioticsdetectedinwatersamplescollectedforthisstudyaresummarizedintable4.(The results of all antibiotic analyses are listed in appendix 1, table 1–2.)Ofthe49targetedantibioticcompounds,12(24percent)weredetectedatleastonetimeforatotalof61detectionsoverall(fig.4;table4;appendix1,table1–2).Thesecompoundsweretrimethoprim,lincomycin,iso-chlorotetracycline,sulfamethoxazole,sulfa-methazine,ofloxacin,ciprofloxacin,tylosin,roxithromycin,erythromycin-H2O,erythromycin,andazithromycin(fig.4).Theconcentrationsofcompoundsdetectedrangedfrom0.005to0.140µg/Lwithamedianvalueof0.014µg/L(fig.4).Antibioticcompounddetectionsweresimilartothosedetectedinthreepreviousantibioticstudies:FurlongandBoyd,2002(erythromycin,sulfamethoxazole,andtrimethoprim);Roweandothers,2004(lincomycinanderythromycin-H2O);andKolpinandothers,2002(trimethoprim,lincomycin,sulfa-methoxazole,sulfamethazine,ciprofloxacin,roxithromycin,erythromycin-H2O,andtylosin).Macrolidesandsulfonamideswerethemostcommonlydetectedantibioticgroupsrepre-senting41percent(25)and28percent(17)ofalldetections,respectively(fig.5).Huangandothers(2001)suggestedthatsulfonamides,quinolines,andmacrolidesarelikelywatercontaminantsbecausetheylackstrongsedimentsorptionpropertiesandthusaremorelikelytobefoundinthewatercolumnthaninsediment.Azithromycin(9detections)wasmostfrequentlydetectedmacrolide,andsulfamethoxazole(16detections)wasthemostcommonlydetectedsulfonamide(figs.4and6).Onlyonetetracyclinecompoundwasdetected,iso-chlorotetracycline,adegradateproductofchlorotetra-cycline(figs.4and6).Huangandothers(2001)notedthattetracyclinesmaypersistforasignificantperiodoftimebutarelessmobilethanotherantibioticgroups,owingtosorptiontosoil.Theantibioticgroup“other”had12totaldetections;lincomycinandtrimethoprimwerebothdetected6times(figs.5and6).Ciprofloxacin(2detections)andofloxacin(3detections)weretheonlyquinolinesdetectedinthestudyarea(figs.4and6).Nobetalactamsweredetected(fig.5).Previousstudiesalsoindicatethatbetalactamsgenerallyundergohydrolysisfairlyquicklyundermildlyacidicorbasicconditions(Huangandothers,2001);thus,betalactamsarenotlikelytopersistunderpHconditionstypicaloftheSciotoRiverBasin(appendix1,table1–1).

Sulfamethoxazole,anantibioticcompoundthatisoftenusedincombinationwithotherantibioticstotreatinfections,hadthesinglehighestconcentrationat0.14µg/L(fig.6).Sul-famethoxazolebiodegradesslowlyifatall,andsulfonamides,ingeneral,exhibitweaksorptiontosoils.Inaddition,hydroly-sisofsulfonamidesataneutralpHrangeisveryslowandcanbeconsiderednegligible,makingthemmorelikelytopersistinsolution(Huangandothers,2001).

At least one antibiotic was detected at 11 of the 12 sites; Hap Cremean F was the only site with no antibiotic detections (fig. 7). SciotoRivernearProspecthadthemostdetectionsoverallat17andthemostdetections(7)onanyonesamplingdate(onDecember8,2005).TheSciotoRiverdownstreamfromCW-104hadatotalof16detections.Bothsiteshadnolessthanthreeantibioticcompoundsdetectedduringallsamplingevents.PowderLickRunnearSummersville,asmallintermittentstream,hadtracedetectionsoflincomycin,agrowthpromoterinlivestock.Thiscouldbeapossiblecon-nectiontothepresenceofCAFOsupstreamfromthesamplingsiteorotheragriculturalusesinthewatershed(fig.2).

Onlytwoantibiotics,sulfamethoxazoleandazithromy-cin,weredetectedattheHapCremeanandParsonsAvenueWTPs,source-waterintakesites(fig.7).TheDublinRoadWTPsource-waterintakesitehadthemostantibioticsidenti-fied(6)foranyonesamplingevent(May24,2006)andalsohaddetectionsforallfoursamplingevents;moreover,itislocatedbetweenSciotoRivernrProspectandSciotoRiverdownstreamCW-104,bothofwhichhadnumerousdetections(17and16,respectively;figs.3and7).Thefinished-watersiteattheParsonsAvenueWTPhaddetectionsofazithromycin,roxithromyocinandtylosin,whereasHapCremeanhadnone.TheDublinRoadWTPfinished-watersite(DublinRoadF)hadonedetection(azithromycin)intheDecember2005sample.Detentiontimesforwater-treatmentprocesseswerenotincludedinthesamplingprotocol;therefore,conclusionsabouttheefficiencyoftheWTPswerenotdrawn.

Datafromsurface-watersiteswereevaluatedtodeter-minepotentialseasonalvariationsinoccurrenceandconcen-trations(fig.8).Thenumberofantibioticdetectionsdecreasedfromwinter(31)tosummer(6)androseslightlyinthefall(9).Thewintersample(December2005)yieldedjustover50per-centofthetotaldetectionsforthisinvestigationinarelativelylow-flowsetting.Alloftheantibioticsdetectedduringthecourseofthisinvestigation(exceptforiso-chlorotetracycline)weredetectedinatleastonewatersamplecollectedduringtheDecember2005samplingevent.Otherantibioticstudies(Fur-longandBoyd,2002)alsohavedocumentedalargenumberofdetectionsinthecoolestmonths.FurlongandBoyd(2002)suggestedthatwarmwatertemperaturesfoundinthesum-mermonthscauseanincreaseinbiologicalactivityandmaysignificantlyincreasethedegradationorbiologicaluptakeofsomecompounds.Inaddition,Huangandothers(2001)foundthattetracyclinesandquinolinesaresusceptibletophotodeg-radation,whichmayexplainwhytheyweredetectedinthecoolfallthroughspringmonthsofshorterphotoperiodsandinterference(shadingfromiceandfallenleaves)andnotinthesummer.Theconcentrationsofantibioticcompoundswereonlyslightlyhigherinthespringandsummersamplesthaninthefallandwintersamples.Hydrologicconditionsweremixed(relativelylowandhighflows)duringthesamplingperiodsforboththespringandsummerandthefallandwinter.Gallowayandothers(2005)suggestedapositiverelationbetweenwatertemperatureandantibioticconcentrationduetomobilizationofcertain antibioticcompounds.


Table 4. Total numbers of detections of antibiotic compounds in source- and finishedwater sites from the Scioto River Basin, Ohio, 2005–6.

[Allvaluesareinmicrogramsperliter; bold typeindicatescompoundsthatweredetectedatleastonce]

ConstituentDetection

levelNumber of detections

ConstituentDetection

levelNumber of detections

Beta lactams Tetracyclines and degradation products

Amoxicillin <0.010 0 Chlorotetracycline <0.010 0

Ampicillin <0.010 0 Anhydro-Chlorotetracycline <0.010 0

Cefotaxime <0.010 0 Epi-anhydro-Chlorotetracycline <0.010 0

Cloxacillin <0.010 0 Epi-chlorotetracycline <0.010 0

Oxacillin <0.010 0 Epi-iso-Chlorotetracycline <0.010 0

PenicillinG <0.010 0 Iso-Chlorotetracycline <0.010 1

PenicillinV <0.010 0 Demeclocycline <0.010 0

Macrolides and degradation products Doxycycline <0.010 0

Azithromycin <0.005 9 Minocycline <0.010 0

Erythromycin <0.005 7 Oxytetracycline <0.010 0

Erythromycin-H20 <0.005 6 Alphaapo-oxytetracycline <0.010 0

Roxithromycin <0.005 2 Betaapo-oxytetracycline <0.010 0

Tylosin <0.005 1 Epi-oxytetracycline <0.010 0

Virginiamycin <0.005 0 Tetracycline <0.010 0

Quinolines Anhydro-tetracycline <0.010 0

Ciprofloxacin <0.005 2 Epi-anhydro-tetracycline <0.010 0

Clinafloxacin <0.005 0 Epi-tetracycline <0.010 0

Flumequine <0.005 0 Other antibiotics

Lomefloxacin <0.005 0 Carbadox <0.005 0

Norfloxacin <0.005 0 Lincomycin <0.005 6

Oxfloxacin <0.005 3 Ormetoprim <0.005 0

OxolinicAcid <0.005 0 Trimethoprim <0.005 7

Sarafloxacin <0.005 0

Sulfonamides

Sulfachlorpyradazine <0.005 0

Sulfadiazine <0.005 0

Sulfadimethoxine <0.005 0

Sulfamerazine <0.005 0

Sulfamethazine <0.005 1

Sulfamethoxazole <0.005 16

Sulfathiazole <0.005 0

X

EXPLANATION

Percentile—Percentage of analyses equal to or less than indicated values 90th percentile

75th percentile

50th percentile (median)

25th percentile

10th percentile X Outlier (extreme value) Mean

Quinolines Tetracyclines and degradation products Macrolides and degradation products Sulfonamides Other antibiotics

Interquartile range

DET

ECTI

ON

FRE

QU

ENCY

CONCENTRATION, IN MICROGRAMS PER LITER1E-3 0.01 0.1 1

TrimethoprimOrmetoprim

LincomycinCarbadox

Epi-tetracyclineEpi-anhydro-tetrcycline

Anhydro-tetracyclineTetracycline

Epi-oxytetracyclineBeta apo-oxytetracycline

Alpha apo-oxytetracyclineOxytetracycline

MinocyclineDoxycycline

DemeclocyclineIso-chlororotetracycline

Epi-iso-chlorotetracyclineEpi-chlorotetracycline

Epi-anhydro-ChlorotetracyclineAnydro-Chlorotetracycline

ChlorotetracyclineSulfathiazole

SulfamethoxazoleSulfamethazine

SulfamerazineSulfadimethoxine

SulfadiazineSulfachlorpyradazine

Sara�oxacinOxolinic Acid

O�oxacinNor�oxacin

Lome�oxacinFlumequine

Clina�oxacinCipro�oxacinVirginiamycin

TylosinRoxithromycin

Erthyromycin-H20ErythromycinAzithromycin

Penicillin VPenicillin G

OxacillinCloxacillin H20

CefotaximeAmpicillin

Amoxicillin

23.115.4

15.4

17.9

5.1

5.1

7.7

2.6

2.6

41

2.6

17.9


Figure 4. Occurrence and concentrations of antibiotic compounds at sites in the upper Scioto River Basin, Ohio, and corresponding detection frequencies evaluated against each compound’s miminum reporting level.

Quinolines n=5

(8 percent)

Sulfonamidesn=17

(28 percent)

Macrolidesn=25

(41 percent)

Other n=13

(21 percent)

Tetracyclinesn=1

(2 percent)

0.027

0.018

0.08

Surface-water sites, including intake sources (8)

Finished-water sites (3)

Groundwater sites (1)

Maximum concentration(micrograms per liter)0.14

20

15

10

5

0

0.026

Azith

rom

ycin

Tylo

sin

Eryt

hrom

ycin

-H20

Num

ber o

f det

ectio

ns

Eryt

hrom

ycin

Roxit

hrom

ycin

Cipr

o�ox

acin

O�ox

acin

Sulfa

met

hazin

e

Sulfa

met

hoxa

zole

Iso-c

hlor

otet

racy

cline

Linco

myc

in

Trim

etho

prim

0.046

0.009 0.009

0.006 0.037

0.013

0.016

0.14


Figure 5. Total number of detections (61) by antibiotic group for collection sites in the upper Scioto River Basin, 2005–6 (n, number of detections; beta lactams were not detected).

Figure 6. Summary of antibiotic compounds detected in water samples collected from the upper Scioto River Basin, Ohio, 2005–6.

Scioto River DS from CW-104

Scioto River near Prospect

Big Walnut Creek at Sunbury

Powder Lick Run near Somersville

Columbus Well Field CW-101

Dublin Road WTP, I

Dublin Road WTP, F

Hap Creman WTP, I

Hap Creman WTP, F

Parsons Avenue WTP, I

Parsons Avenue WTP, FNDND

NDND

NDNDND

NDNDND

ND

NDND

NDND

ND

NDND

5/22/2006

5/22/2006

5/23/2006

5/23/2006

5/25/2006

5/24/2006

5/24/2006

5/24/2006

5/24/2006

5/24/2006

5/25/2006

5/25/2006

8/22/2006

8/23/2006

8/23/2006

8/22/2006

8/22/2006

10/18/2006

10/18/2006

10/18/2006

10/19/2006

10/24/2006

10/24/2006

10/24/2006

10/24/2006

10/23/2006

10/23/2006

10/19/2006

12/8/2005

12/8/2005

12/6/2005

12/6/2005

12/7/2005

12/7/2005

12/7/2005

12/7/2005

12/7/2005

12/6/2005

12/6/2005

DAT

E O

F SA

MPL

E CO

LLEC

TIO

N

NUMBER OF DETECTIONS0 1 2 3 4 5 6 7 8 9 10

EXPLANATION Groundwater Source waters from WTP Surface water Finished waters from WTP


Figure 7. Numbers of detections of antibiotic compounds by sampling site and date in source and finished waters of the upper Scioto River Basin, central Ohio, 2005–6.


Figure 8. Total number of detections at all sites, by season, in the upper Scioto River Basin, central Ohio, 2005–6.

Comparing results from the previous study to those from this study, the antibiotic analysis method used during 2001 included just over half (26) of the antibiotic compounds tested for in 2005–6 (49). In addition, four of the compounds analyzed for in 2001 were not analyzed for in 2005–6, and the minimum reporting limits (MRLs) ranged from twice to an order of magnitude higher than the current laboratory MRLs. Not surprisingly, many of the compounds detected in

the earlier investigations were the same as those detected in this report (fig. 1). It is important to note that the number of antibiotic compounds reported in 2001 (3) was far fewer than the compounds reported in 2005–6 (61). It is expected that lower MRLs and an expanded compound analysis list, such as the ones used in this study, would yield higher detection frequencies.

References Cited 15

Summary and Conclusions

Occurrenceofantibioticcompoundsinsurface-and-groundwaterhasbeenatopicofincreasinginterest,alongwiththeunderstandingoffate(ortransport)ofthesecom-poundsandthepossiblehealtheffectsinhumansandaquaticlife.TheU.S.GeologicalSurvey,incooperationwiththeCityofColumbus,DivisionofPowerandWater,collectedwatersamplesfromlocationsintheupperSciotoRiverBasinfromDecember2005toOctober2006todeterminetheoccur-renceanddistributionofantibioticcompoundsinsourcewaterfromtheCityofColumbus,Ohio.Sampleswerecollectedfromfivesurface-watersites,onegroundwatersite,andtwosites—asource-andfinished-watersite—ateachofthreewater-treatmentplants(WTPs).Inanefforttotargetworst-caseconditions,sampleswerecollectedduringperiodswhenresultsofdailynitrateandpesticidemonitoringdonebytheColumbusDivisionofPowerandWaterindicatedthatcon-centrationsofagrochemicalswerehighestinthesourcewater.Low-flowsampleswerecollectedinlatesummerinanefforttotargetperiodswhentreatedwastewaterandseptic-tankdis-chargelikelyrepresentalargerproportionofthetotalstream-flow.Thequality-control(QC)procedures,whichconsistedofcollectingandanalyzingfieldblanksandreplicates,followedageneralquality-assurance/qualitycontrolprotocolestablishedforlow-levelorganicanalyses.Antibioticfieldblanksamplesrepresentedabout15percentoftheenvironmentalsamplesandyieldednodetections.Tworeplicatesampleswerecol-lectedatstudysitesColumbusWellFieldCW-101andPowderLickRunnearSummersville,Ohio.Thereplicatesindicatedgoodreproducibilityoflaboratoryresultswithanidenticalconcentrationof(0.005µg/L)forlincomycin.

Ofthe49targetedantibioticcompounds,12(24percent)weredetectedatleastonetimeforatotalof61detections.Thesecompoundsweretrimethoprim,lincomycin,iso-chlo-rotetracycline,sulfamethoxazole,sulfamethazine,ofloxacin,ciprofloxacin,tylosin,roxithromycin,erythromycin-H2O,erythromycin,andazithromycin.Sulfamethoxazole,ananti-bioticcompoundthatisoftenusedincombinationwithotherantibioticstotreatinfections,hadthesinglehighestconcen-trationat0.14µg/L.Azithromycin(9detections)wasmostfrequentlydetectedmacrolideandsulfamethoxazole(16detec-tions)wasthemostcommonlydetectedsulfonamide.Atleastoneantibioticwasdetectedat11ofthe12sites;HapCremeanFwastheonlysitewithnoantibioticdetections.SciotoRivernearProspecthadthemostdetectionsoverallat17andthemostdetections(7)onanyonesamplingdate(onDecember8,2005).TheSciotoRiverdownstreamfromCW-104hadatotalof16detections.Datafromsurface-watersiteswereevaluatedtodeterminepotentialseasonalvariationsinoccurrenceandconcentrations.Thenumberofantibioticdetectionsdecreasedfromwinter(31)tosummer(6)androseslightlyinthefall(9).Thewintersample(December2005)yieldedjustover50per-centofthetotaldetectionsforthisinvestigationinarelativelylow-flowsetting.

Throughoutthedurationofthisproject,knowledgeofcollection,processing,andanalysisoforganicwastewatercontaminantshavecontinuedtoevolveandimprove.Time-integratedsourceandfinished-watersamplescollectedovera24-hourperiodwithcalculatedresidencetimebetweenthesourceandfinishedwouldbeapreferredcollectionmethodcomparedtoagrabsampleforwater-treatmentplants.Allow-ingforresidencetimeinthetreatmentprocesswouldprovideamorethoroughevaluationofoccurrenceanddistributionandwouldalsoimproveunderstandingofdrinking-watertreatmentprocessesandpersistenceofmeasurableconcentrationsoforganicwastewatercontaminantsinfinishedwater.

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Casewell,Mark;Friis,Christian;Marco,Enrico;McMullin,Paul;andPhillips,Ian,2003,TheEuropeanbanongrowth-promotingantibioticsandemergingconsequencesforhumanandanimalhealth:JournalofAntimicrobialChemo-therapy,v.52,no.2,p.159–161.

Cižman,Milan;Pokorn,Marko;Seme,Katja;Oražem,Andreja;andParagi,Metka,2001,Therelationshipbetweentrendsinmacrolideuseandresistancetomacrolidesofcommonrespiratorypathogens:JournalofAntimicrobialChemotherapy,v.47,no.4,p.475–477.

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Halling-Sørensen,B.;Nielson,S.N.;Lanzky,P.F.; Inger-slev, F.; Holten Lützhoft, H.C.; and Jorgensen, S.E.,1998,Occurrence, fate and effects of pharmaceuticalsubstancesintheenvironment—A review: Chemosphere, v.35, no.2,p.357–393.

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http://pubs.water.usgs.gov/twri9A4/

17

Appendixes 1–2

Appendix 1. Water-Quality Analyses and Quality-Control Tests

Appendix 2. Sample Analysis


Table 1–1. Field parameters from sampling locations in the upper Scioto River Basin, Ohio, 2005–6.—Continued

[ft3/s,cubicfeetpersecond;µS/cm,microsiemenspercentimeterat25degreesCelsius;mg/L,milligramsperliter;ºC,degreesCelsius;mmHg,millimetersofmercury;—,notmeasured;<,lessthan;WTP,water-treatmentplant;DS,downstream;CW,collectorwell;F,finishedwater;I,intake]

Site nameDate of sample

collectionTime

Discharge(ft3/s)

Water temperature

(ºC)

Airtemperature

(ºC)

Specific conductance,

field (µS/cm)

pH,(standard

units)

Dissolved oxygen(mg/L)

Barometric pressure

(mm of Hg)

SciotoRivernearProspect

12/082005 1030 203 0.2 -4.0 837 8.08 14.2 746

05/23/2006 1140 340 15.29 20 699 7.87 8.3 744

08/23/2006 1145 44 23.5 23.6 788 7.97 10.1 742

10/18/2006 1200 1910 12.07 14 340 7.53 6.45 739

DublinRoadWTP,F

12/07/2005 1035 — — — 483 8.05 — —

05/24/2006 0935 — — — 596 7.85 — —

08/22/2006 1325 — — — 506 7.97 — —

10/24/2006 1005 — — — 396 7.73 — —

DublinRoadWTP,I

12/07/2005 1040 — — — — — — —

05/24/2006 0945 — — — 658 7.74 — —

08/22/2006 1320 — — — 536 7.7 — —

10/24/2006 1000 — — — 423 7.82 — —

MillCreekbelowMarysville

12/08/2005 1215 15.7 0 -2 702 8.35 15.9 746

05/22/2006 1200 21.8 14.9 16 669 8.23 7.1 740

08/23/2006 1000 0 20.6 23.5 1011 7.71 7.3 742

10/19/2006 1015 126 14 13.2 498 7.8 8.74 733

PowderLickRunnearSummersville

05/22/2006 1000 0.26 13.1 13 982 7.83 7.77 740

08/22/2006 1015 0 18.8 24.9 1476 7.44 5.61 742

10/18/2006 0930 11.4 12.4 11.5 407 7.7 7.55 735

Appendix 1. Water-Quality Analyses and Quality-Control Results

Appendix 1. Water-Quality Analyses and Quality-Control Results 19

Table 1–1. Field parameters from sampling locations in the upper Scioto River Basin, Ohio, 2005–6.—Continued

[ft3/s,cubicfeetpersecond;µS/cm,microsiemenspercentimeterat25degreesCelsius;mg/L,milligramsperliter;ºC,degreesCelsius;mmHg,millimetersofmercury;—,notmeasured;<,lessthan;WTP,water-treatmentplant;DS,downstream;CW,collectorwell;F,finishedwater;I,intake]

Site nameDate of sample

collectionTime

Discharge(ft3/s)

Water temperature

(ºC)

Airtemperature

(ºC)

Specific conductance,

field (µS/cm)

pH,(standard

units)

Dissolved oxygen(mg/L)

Barometric pressure

(mm of Hg)

HapCremeanWTP,I

12/07/2005 1120 — — — 384 8.1 — —

05/24/2006 1010 — — — 410 7.89 — —

10/24/2006 1035 — — — 379 8.33 — —

HapCremeanWTP,F

12/07/2005 1115 — — — 340 8.14 — —

05/24/2006 1015 — — — 322 7.38 — —

10/24/2006 1040 — — — 329 8.11 — —

SciotoRiverDSfromCW-104

12/06/2005 1130 1840 7.3 -3.0 671 8.1 — 745

05/23/2006 1400 1370 17.1 23 706 8.2 10.2 752

10/19/2006 1315 7460 13.82 16 608 7.87 9.93 740

BigWalnutCreekatSunbury

12/08/2005 0915 25 0 -9.0 701 8.27 15.8 746

05/23/2006 1000 49 12.3 14 529 8.22 10.61 744

10/18/2006 1330 447 13.11 17.5 363 7.75 9.98 739

ColumbusWellFieldCW-101

12/06/2005 1055 — — — 781 7.5 — —

05/25/2006 1010 — — — 829 7.3 — —

ParsonsAvenueWTP,I

12/06/2005 1020 — — — 867 7.24 — —

05/25/2006 0940 — — — 861 7.09 — —

10/23/2006 1310 — — — 882 7.5 — —

ParsonsAvenueWTP,F

12/06/2005 1015 — — — 560 7.8 — —

05/23/2006 0945 — — — 554 7.46 — —

10/23/2006 1315 — — — 536 7.7 — —


Table 1–2. Water-quality analyses from sampling locations in the upper Scioto River Basin, Ohio, 2005–6.—Continued

[µg/L,microgramsperliter;<,lessthan;WTP,water-treatmentplant;F,finishedwater;I,intake;CW,collectorwell;DS,downstream;bold,valueexceededdetectionorreportinglevel]

Site name Date Time Lincomycin Carbadox Trimethoprim Ormetoprim TetracyclineAnhydro-

tetracyclineEpi-

tetracycline


12/08/2005 1030 <0.005 <0.005 0.012 <0.005 <0.010 <0.010 <0.010

05/23/2006 1140 <0.005 <0.005 0.006 <0.005 <0.010 <0.010 <0.010

08/23/2006 1145 <0.005 <0.005 0.006 <0.005 <0.010 <0.010 <0.010

10/18/2006 1200 0.018 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

DublinRoadWTP,F

12/07/2005 1035 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

05/24/2006 0935 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

08/22/2006 1325 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

10/24/2006 1005 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

DublinRoadWTP,I

12/07/2005 1040 0.007 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

05/24/2006 0945 0.006 <0.005 0.021 <0.005 <0.010 <0.010 <0.010

08/22/2006 1320 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

10/24/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010


12/08/2005 1215 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

05/22/2006 1200 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

08/23/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

10/19/2006 1015 0.010 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010


05/22/2006 1000 0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

08/22/2006 1015 0.008 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

10/18/2006 0930 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010




Site name Date Time Lincomycin Carbadox Trimethoprim Ormetoprim TetracyclineAnhydro-

tetracyclineEpi-

tetracycline

HapCremeanWTP,I

12/07/2005 1120 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

05/24/2006 1010 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

10/24/2006 1035 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

HapCremeanWTP,F

12/07/2005 1115 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

05/24/2006 1015 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

10/24/2006 1040 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010


12/06/2005 1130 <0.005 <0.005 0.027 <0.005 <0.010 <0.010 <0.010

05/23/2006 1400 <0.005 <0.005 0.027 <0.005 <0.010 <0.010 <0.010

10/19/2006 1315 <0.005 <0.005 0.008 <0.005 <0.010 <0.010 <0.010


12/08/2005 0915 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

05/23/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

10/18/2006 1330 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010


12/06/2005 1055 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

05/25/2006 1010 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

ParsonsAvenueWTP,I

12/06/2005 1020 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

05/25/2006 0940 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

10/23/2006 1310 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

ParsonsAvenueWTP,F

12/06/2005 1015 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

05/25/2006 0945 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

10/23/2006 1315 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010




Site name Date TimeEpi-

anhydro- tetracycline

Chloro- tetracycline

Anhydro- chloro-

tetracycline

Epi- anhydro-chloro-

tetracycline

Epichloro-tetracycline

Isochloro-tetracycline

Epi- isochloro-

tetracycline


12/08/2005 1030 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 1140 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/23/2006 1145 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/18/2006 1200 <0.010 <0.010 <0.010 <0.010 <0.010 0.037 <0.010

DublinRoadWTP,F

12/07/2005 1035 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 0935 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/22/2006 1325 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1005 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

DublinRoadWTP,I

12/07/2005 1040 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 0945 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/22/2006 1320 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


12/08/2005 1215 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/22/2006 1200 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/23/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/19/2006 1015 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


05/22/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/22/2006 1015 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/18/2006 0930 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010




Site name Date TimeEpi-

anhydro- tetracycline

Chloro- tetracycline

Anhydro- chloro-

tetracycline

Epi- anhydro-chloro-

tetracycline

Epichloro-tetracycline

Isochloro-tetracycline

Epi- isochloro-

tetracycline

HapCremeanWTP,I

12/07/2005 1120 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 1010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1035 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

HapCremeanWTP,F

12/07/2005 1115 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 1015 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1040 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


12/06/2005 1130 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 1400 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/19/2006 1315 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


12/08/2005 0915 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/18/2006 1330 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


12/06/2005 1055 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/25/2006 1010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

ParsonsAvenueWTP,I

12/06/2005 1020 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/25/2006 0940 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/23/2006 1310 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

ParsonsAvenueWTP,F

12/06/2005 1015 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/25/2006 0945 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/23/2006 1315 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010




Site name Date TimeDeme-

clocyclineOxy-

tetracycline

Alphaapoxy-

tetracycline

Betaapoxy-

tetracycline

Epioxy-tetracycline

Minocycline Doxycycline


12/08/2005 1030 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 1140 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/23/2006 1145 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/18/2006 1200 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

DublinRoadWTP,F

12/07/2005 1035 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 0935 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/22/2006 1325 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1005 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

DublinRoadWTP,I

12/07/2005 1040 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 0945 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/22/2006 1320 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


12/08/2005 1215 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/22/2006 1200 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/23/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/19/2006 1015 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


05/22/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/22/2006 1015 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/18/2006 0930 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010




Site name Date TimeDeme-

clocyclineOxy-

tetracycline

Alphaapoxy-

tetracycline

Betaapoxy-

tetracycline

Epioxy-tetracycline

Minocycline Doxycycline

HapCremeanWTP,I

12/07/2005 1120 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 1010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1035 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

HapCremeanWTP,F

12/07/2005 1115 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 1015 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1040 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


12/06/2005 1130 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 1400 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/19/2006 1315 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


12/08/2005 0915 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/18/2006 1330 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


12/08/2005 1055 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/25/2006 1010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

ParsonsAvenueWTP,I

12/06/2005 1020 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/25/2006 0940 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/23/2006 1310 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

ParsonsAvenueWTP,F

12/06/2005 1120 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/25/2006 1010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/23/2006 1315 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010




Site name Date Time SulfathiazoleSulfa-

merazineSulfa-

methazineSulfa-

methoxazole

Sulfa-chlor-

pyradazine

Sulfa-dimethoxine

Sulfadiazine


12/08/2005 1030 <0.005 <0.005 <0.005 0.050 <0.005 <0.005 <0.005

05/23/2006 1140 <0.005 <0.005 <0.005 0.024 <0.005 <0.005 <0.005

08/23/2006 1145 <0.005 <0.005 <0.005 0.140 <0.005 <0.005 <0.005

10/18/2006 1200 <0.005 <0.005 <0.005 0.013 <0.005 <0.005 <0.005

DublinRoadWTP,F

12/07/2005 1035 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 0935 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/22/2006 1325 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

DublinRoadWTP,I

12/07/2005 1040 <0.005 <0.005 0.006 0.022 <0.005 <0.005 <0.005

05/24/2006 0945 <0.005 <0.005 <0.005 0.031 <0.005 <0.005 <0.005

08/22/2006 1320 <0.005 <0.005 <0.005 0.017 <0.005 <0.005 <0.005

10/24/2006 1000 <0.005 <0.005 <0.005 0.012 <0.005 <0.005 <0.005


12/08/2005 1215 <0.005 <0.005 <0.005 0.010 <0.005 <0.005 <0.005

05/22/2006 1200 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/23/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/19/2006 1015 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


05/22/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/22/2006 1015 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/18/2006 0930 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005




Site name Date Time SulfathiazoleSulfa-

merazineSulfa-

methazineSulfa-

methoxazole

Sulfa-chlor-

pyradazine

Sulfa-dimethoxine

Sulfadiazine

HapCremeanWTP,I

12/07/2005 1120 <0.005 <0.005 <0.005 0.008 <0.005 <0.005 <0.005

05/24/2006 1010 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1035 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

HapCremeanWTP,F

12/07/2005 1030 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 1140 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1200 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


12/06/2005 1130 <0.005 <0.005 <0.005 0.088 <0.005 <0.005 <0.005

05/23/2006 1400 <0.005 <0.005 <0.005 0.052 <0.005 <0.005 <0.005

10/19/2006 1315 <0.005 <0.005 <0.005 0.074 <0.005 <0.005 <0.005


12/08/2005 0915 <0.005 <0.005 <0.005 0.016 <0.005 <0.005 <0.005

05/23/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/18/2006 1330 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


12/06/2005 1055 <0.005 <0.005 <0.005 0.006 <0.005 <0.005 <0.005

05/25/2006 1010 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

ParsonsAvenueWTP,I

12/06/2005 1020 <0.005 <0.005 <0.005 0.005 <0.005 <0.005 <0.005

05/23/2006 0940 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/25/2006 1310 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

ParsonsAvenueWTP,F

12/06/2005 1015 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/25/2006 0945 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/23/2006 1315 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005




Site name Date Time NorfloxacinCipro-

floxacinClina-

floxacinFlumequine

Lome- floxacin

OfloxacinOxolinic

Acid


12/08/2005 1030 <0.005 0.006 <0.005 <0.005 <0.005 0.01 <0.005

05/23/2006 1140 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/23/2006 1145 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/18/2006 1200 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

DublinRoadWTP,F

12/07/2005 1035 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 0935 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/22/2006 1325 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

DublinRoadWTP,I

12/07/2005 1040 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 0945 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/22/2006 1320 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


12/08/2005 1215 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/22/2006 1200 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/23/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/19/2006 1015 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


05/22/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/22/2006 1015 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/18/2006 0930 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005




Site name Date Time NorfloxacinCipro-

floxacinClina-

floxacinFlumequine

Lome- floxacin

OfloxacinOxolinic

Acid

HapCremeanWTP,I

12/07/2005 1120 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 1010 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1035 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

HapCremeanWTP,F

12/07/2005 1030 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 1140 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1200 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


12/06/2005 1130 <0.005 0.009 <0.005 <0.005 <0.005 0.013 <0.005

05/23/2006 1400 <0.005 <0.005 <0.005 <0.005 <0.005 0.009 <0.005

10/19/2006 1315 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


12/08/2005 0915 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/23/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/18/2006 1330 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


12/06/2005 1055 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/25/2006 1010 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

ParsonsAvenueWTP,I

12/06/2005 1020 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/23/2006 0940 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/25/2006 1310 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

ParsonsAvenueWTP,F

12/06/2005 1015 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/25/2006 0945 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/23/2006 1315 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005




Site name Date Time Sarafloxacin Azithromycin TylosinVirginia-

mycinErythromycin-

H20Erythromycin

Roxithro- mycin


12/08/2005 1030 <0.005 0.011 <0.005 <0.005 0.014 0.015 <0.005

05/23/2006 1140 <0.005 <0.005 <0.005 <0.005 <0.005 0.007 <0.005

08/23/2006 1145 <0.005 <0.005 <0.005 <0.005 0.013 0.022 <0.005

10/18/2006 1200 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

DublinRoadWTP,F

12/07/2005 1035 <0.005 0.025 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 0935 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/22/2006 1325 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

DublinRoadWTP,I

12/07/2005 1040 <0.005 0.031 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 0945 <0.005 <0.005 <0.005 <0.005 0.017 0.010 0.009

08/22/2006 1320 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


12/08/2005 1215 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/22/2006 1200 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/23/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/19/2006 1015 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


05/22/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

08/22/2006 1015 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/18/2006 0930 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005




Site name Date Time Sarafloxacin Azithromycin TylosinVirginia-

mycinErythromycin-

H20Erythromycin

Roxithro- mycin

HapCremeanWTP,I

12/07/2005 1120 <0.005 0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 1010 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1035 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

HapCremeanWTP,F

12/07/2005 1030 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

05/24/2006 1140 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/24/2006 1200 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


12/06/2005 1130 <0.005 0.036 <0.005 <0.005 0.021 0.019 <0.005

05/23/2006 1400 <0.005 <0.005 <0.005 <0.005 0.026 0.046 <0.005

10/19/2006 1315 <0.005 <0.005 <0.005 <0.005 0.007 0.008 <0.005


12/08/2005 0915 <0.005 0.008 <0.005 <0.005 <0.005 <0.005 <0.005

05/23/2006 1000 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/18/2006 1330 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


12/06/2005 1055 <0.005 0.048 <0.005 <0.005 <0.005 <0.005 <0.005

05/25/2006 1010 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

ParsonsAvenueWTP,I

12/06/2005 1020 <0.005 0.043 <0.005 <0.005 <0.005 <0.005 <0.005

05/23/2006 0940 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/25/2006 1310 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

ParsonsAvenueWTP,F

12/06/2005 1015 <0.005 0.080 0.016 <0.005 <0.005 <0.005 0.023

05/25/2006 0945 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

10/23/2006 1315 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005




Site name Date Time Amoxicillin Ampicillin Cefotaxime Cloxacillin Oxacillin Penicillin G Penicillin V


12/08/2005 1030 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 1140 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/23/2006 1145 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/18/2006 1200 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

DublinRoadWTP,F

12/07/2005 1035 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 0935 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/22/2006 1325 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1005 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

DublinRoadWTP,I

12/07/2005 1040 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 0945 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/22/2006 1320 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


12/08/2005 1215 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/22/2006 1200 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/23/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/19/2006 1015 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010


05/22/2006 1000 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

08/22/2006 1015 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/18/2006 0930 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010




Site name Date Time Amoxicillin Ampicillin Cefotaxime Cloxacillin Oxacillin Penicillin G Penicillin V

HapCremeanWTP,I

12/07/2005 1120 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 1010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1035 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010

HapCremeanWTP,F

12/07/2005 1030 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

05/24/2006 1140 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

10/24/2006 1200 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010


12/06/2005 1130 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 1400 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

10/19/2006 1315 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010


12/08/2005 0915 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 1000 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

10/18/2006 1330 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010


12/06/2005 1055 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

05/25/2006 1010 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

ParsonsAvenueWTP,I

12/06/2005 1020 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

05/23/2006 0940 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

10/25/2006 1310 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

ParsonsAvenueWTP,F

12/06/2005 1015 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

05/25/2006 0945 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010

10/23/2006 1315 <0.005 <0.005 <0.010 <0.010 <0.010 <0.010 <0.010


Table 1–3. Quality-control analyses from sampling locations in the upper Scioto River Basin, Ohio, 2005–6.

[Allconstituentconcentrationsinmicrogramsperliter;—,notmeasured;<,lessthan;WTP,water-treatmentplant;DS,downstream;CW,collectorwell;F,finishedwater;I,intake;bold,valueexceededdetectionorreportinglevel]

Site name Date Time Lincomycin CarbadoxTri-

methoprimOrmetoprim Tetracycline

Anhydro-tetracycline

Epi- anhydro-

tetracycline

Field blanks

DublinRoadWTP,I 12/07/2005 1041 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

PowderLickRunnearSummersville 08/22/2006 1014 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

HapCremeanWTP,F 10/24/2006 1039 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

BigWalnutCreekatSunbury 05/23/2006 0959 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

SciotoRiverDSfromCW-104 05/23/2006 1359 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

ParsonsAvenueWTP,F 05/23/2006 0944 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

Replicates

PowderLickRunnearSummersville 05/22/2006 1001 0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

ColumbusWellFieldCW-101 05/25/2006 1011 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010 <0.010

Table 1–3. Quality-control analyses from sampling locations in the upper Scioto River Basin, Ohio, 2005–6.—Continued


Site name Date TimeChloro-

tetracycline

Anhydro- chloro-

tetracycline

Epi-anhydro-chloro-

tetracycline

Epi-chloro-

tetracycline

Iso- Chloro-

tetracycline

Epi-iso-chloro-tetra-

cycline

Deme- clocycline

Field blanks

DublinRoadWTP,I 12/07/2005 1041 <0.010 <0.010 <0.010 <0.010 <0.01 <0.01 <0.010


HapCremeanWTP,F 10/24/2006 1039 <0.010 <0.010 <0.010 <0.010 <0.01 <0.01 <0.010




Replicates






Site name Date TimeOxy-

tetracycline

Alphaapooxy-

tetracycline

Betaapooxy-

tetracycline

Epioxy- tetracycline

Minocycline Doxycycline Sulfathiazole

Field blanks

DublinRoadWTP,I 12/07/2005 1041 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.005


HapCremeanWTP,F 10/24/2006 1039 <0.010 <0.010 <0.010 <0.010 <0.010 <0.010 <0.005




Replicates




[Allconstituentconcentrationsinmicrogramsperliter;—notmeasured;<,lessthan;WTP,water-treatmentplant;DS,downstream;CW,collectorwell;F,fin-ishedwater;I,intake;bold,valueexceededdetectionorreportinglevel]

Site name Date TimeSulfa-

merazineSulfa-

methazineSulfa-

methoxazole

Sulfa-chlor-

pyradazine

Sulfa-dimethoxine

Sulfadiazine Norfloxacin

Field blanks

DublinRoadWTP,I 12/07/2005 1041 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005


HapCremeanWTP,F 10/24/2006 1039 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005




Replicates





[Allconstituentconcentrationsinmicrogramsperliter;—notmeasured;<,lessthan;WTP,water-treatmentplant;DS,downstream;CW,collectorwell;F,finishedwater;I,intake;bold,valueexceededdetectionorreportinglevel]

Site name Date TimeCipro-

floxacinClina-

floxacinFlumequine

Lome- floxacin

OfloxacinOxolinic

AcidSara-

floxacinAzithro- mycin

Field blanks

DublinRoadWTP,I 12/07/2005 1041 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

PowderLickRunnearSummersville 08/22/2006 1014 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

HapCremeanWTP,F 10/24/2006 1039 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

BigWalnutCreekatSunbury 05/23/2006 0959 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

SciotoRiverDSfromCW-104 05/23/2006 1359 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

ParsonsAvenueWTP,F 05/23/2006 0944 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

Replicates

PowderLickRunnearSummersville 05/22/2006 1001 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005

ColumbusWellFieldCW-101 05/25/2006 1011 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005 <0.005



Site name Date Time Tylosin VirginiamycinErythro-

mycin-H20Erythromycin

Roxithro-mycin

Amoxocillin Ampicillin

Field blanks

DublinRoadWTP,I 12/07/2005 1041 <0.005 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010

PowderLicknearSummersville 08/22/2006 1014 <0.005 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010

HapCremeanWTP,F 10/24/2006 1039 <0.005 <0.005 <0.005 <0.005 <0.005 <0.010 <0.010




Replicates






Site name Date Time Cefotaxime Cloxacillin Oxacillin Penicilln G Penicillin V

Field blanks

DublinRoadWTP,I 12/07/2005 1041 <0.010 <0.010 <0.010 <0.010 <0.010

PowderLickRunnearSummersville 08/22/2006 1014 <0.010 <0.010 <0.010 <0.010 <0.010

HapCremeanWTP,F 10/24/2006 1039 <0.010 <0.010 <0.010 <0.010 <0.010

BigWalnutCreekatSunbury 05/23/2006 0959 <0.010 <0.010 <0.010 <0.010 <0.010

SciotoRiverDSfromCWl-104 05/23/2006 1359 <0.010 <0.010 <0.010 <0.010 <0.010

ParsonsAvenueWTP,F 05/23/2006 0944 <0.010 <0.010 <0.010 <0.010 <0.010

Replicates

PowderLickRunnearSummersville 05/22/2006 1001 <0.010 <0.010 <0.010 <0.010 <0.010

ColumbusWellFieldCW-101 05/25/2006 1011 <0.010 <0.010 <0.010 <0.010 <0.010


Appendix 2. Sample Analysis

andwerepreparedfortheSQandTETmethodbyadding250µLofformicacidto9.75mLofdeionizedwater,andfortheBLMmethodbyadding10mlofa10percentNaClsolu-tionwith0.5percentdiNa-EDTAtoan11-mLcrimptopvial.

Allofthepreparedsampleswereloadedontheonlinesolidphaseextraction(SPE)Triathalonautosampler.Duringanalysis,theonlineSPElineswererinsedwithsolventsandsolutionsconfiguredwiththeTriathalonautosamplerandthehigh-pressuredispenser.Thecartridgeswererinsedimme-diatelypriortoextraction.Avolumeof10mlofsamplewasdrawnintoaTeflonsampleloopanddispensedthroughtheProspektSPEcartridge.

Theantibioticsforeachmethodwereelutedwith750µLofACNandseparatedusingaliquidchromatography(LC)gradientwiththeAandBmobilephaseslistedintable2–1below(Meyerandothers,2007).TheinitialflowratesoftheAandBmobilephasesweredecreasedandcontainedahigherproportionoftheBmobilephasetoassistinelutingthePros-pektSPEcartridge.Duringtheelution,theLCautosamplerinjected20µLoftheinternalstandard.TheisocraticmobilephasewasusedtoincreasetheaqueousphaseinthemobilephasestreamtofocusthecompoundselutedfromtheSPEcartridgeontotheheadoftheLCcolumn.AfterthemobilephaseflowhadpassedthroughtheSPEcartridge,theflowratewasincreasedto0.36mL/min,andtheisocraticpumpflowwasturnedoff.A3.0×150mmLunaC18(2)(Phenonomenex)with3-µmpackingwasusedtoseparatetheantibioticsforeachofthethreemethods.TheLCcolumnwasrinsedfor5minuteswith100percentmobilephaseBattheendofthegradientandthenequilibratedatinitialconditionsfor5min-utesbeforethenextsampleanalysis.

Table 2–1. Mobile phases used in the liquid chromatography/electrospray ionization-mass spectrometry (LC/ESI-MS) techniques for three common antibiotic groups.

[%,percent]

Mobile-phase name

Antibiotic groups

TetracyclinesSulfonamides and

quinolonesMacrolides and

beta lactams

A 0.3%formicacid 0.3%formicacid 5mMNH4-acetate

B 1.0%formicacid Acetonitrile Acetonitrile

Isocratic 0.3%formicacid 0.3%formicacid 5mMNH4-acetate

Sampleswereextractedforthebetalactamandmacro-lides(BLM)andsulfonamidesandquinolines(SQ)methodsusingHLBProspektcartridges(WatersCorp.,Milford,Mass.)andforthetetracyclines(TET)methodusingaproprietaryGlyphosateProspektcartridge(SparkHolland,Emmen,TheNetherlands).Simatonewasusedasaninternalstandardforallthreemethods;thesurrogatestandardswereoleandomycinfortheBLMmethod,nalidixicacidand13C6sulfamethazinefortheSQmethod,andmeclocyclinefortheTETmethod.A1.23ng/µLsolutionoftheinternalstandard,simatone,wasdiluted1:20fortheBLMandSQmethodsand1:40fortheTETmethod.Thedilutedstandardwasaddedtoanamber2-mLchromatographyvialandplacedontheLCautosamplertray.

Sampleswerepreparedforanalysisbypipettinga10-mLaliquotofeachsampleinto11-mLglasscrimp-topvials.FortheBLMandSQmethods,75mLof6.67ng/mlsurrogatesolutionsweremadeupindistilledwater,andfortheTETmethod,ina5%diNa-EDTAsolution;750µLoftherespectivesurrogatewasaddedtoeachsample,standard,andblank.Standardcurveswerepreparedforeachmethodbydilutingtherespective1-ng/µLstandardmixto1ng/mLwithdistilledwater.Standardsolutions,10mLinvolume,werethenmadeatconcentrationsof0.01,0.02,0.05,0.1,0.2,0.5and1.0µg/L.

Aduplicatesample,a0.5-or1.0-µg/Lmatrix-spikedsample,andablankwereanalyzedafterevery10samplesanda1.0µg/Lstandardsolutionafterevery20.Allstandardsolu-tions,blanks,andmatrixspikesweretreatedthesameasthewatersamples.SamplemodifiersolutionswereaddedtoeachsamplebytheonlineSPEautosamplerjustpriortoextraction

Finnegan and others—O

ccurrence of Antibiotic Com

pounds in Source Water and Finished D

rinking Water from

the Upper Scioto River B

asin, Ohio, 2005–6—

SIR 2010–5083

Documents

Occurrence of Antibiotic Compounds in Source Water and