Com parison of Autom ated and Manual Methods for Solid Phase - - PowerPoint PPT Presentation

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Com parison of Autom ated and Manual Methods for Solid Phase - - PowerPoint PPT Presentation

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Com parison of Autom ated and Manual Methods for Solid Phase Extraction of Endocrine Disrupting Chem icals Kirsten E. Studer, Graduate EPA STAR Fellow David A. Reckhow, Professor of Civil and Environmental Engineering Environmental and Water

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Com parison of Autom ated and Manual Methods for Solid Phase Extraction of Endocrine Disrupting Chem icals

Kirsten E. Studer, Graduate EPA STAR Fellow David A. Reckhow, Professor of Civil and Environmental Engineering

Environmental and Water Resource Engineering

Water Resources Research Conference April 7, 2009

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2 Environmental Engineering

Presentation Outline

Endocrine Disrupting Compounds Solid Phase Extraction Methods Instrumentation Method Comparison Cost Comparison Preliminary Results

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3 Environmental Engineering

Endocrine Disrupting Compounds

Emerging group of contaminants Natural and synthetic hormones Variety of reproductive abnormalities and physical deformities

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4 Environmental Engineering

Diethylstilbestrol MW 268 g/ mol Estriol MW 288 g/ mol Estradiol MW 272 g/ mol 17β-Ethinylestradiol MW 296 g/ mol Estrone MW 270 g/ mol

Estrogens

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5 Environmental Engineering

Solid Phase Extraction

Extraction of EDCs from environmental matrixes Method comparison

  • Manual versus

automated

  • EPA 1694 Method:

Pharmaceuticals and Personal Care Products in Water, Soil, Sediment and Biosolids by HPLC/ MS/ MS (2007)

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6 Environmental Engineering

SPE Method Comparison

HLB Oasis cartridges

  • On-line
  • Single use

C-8 analytical column (X-Bridge) LC/ MS/ MS (ESI-)

Parent/ Daughter ( m / z) Cone/ Collision ( V) Estrone (E1) 269.3 / 145.3 50 / 30 Estriol (E3) 287.1 / 171.0 55 / 35 Estradiol (E2) 271.3 / 145.3 50 / 35 17B-Ethinylestradiol (EE2) 295.2 / 145.2 50 / 40 Diethylstilbestrol (DES) 267.1 / 251.2 40 / 25

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7 Environmental Engineering

Manual SPE Method

500 mL to 1000 mL sample size concentrated to 1 mL One-time use HLB extraction cartridges 8 hour extraction method time 16 min instrument run time HPLC-MS/ MS

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8 Environmental Engineering

Manual SPE Method

Approxim ate Minim um Detection Lim its ( MDLs) Estrone (E1) 5 ppt Estriol (E3) 5 ppt Estradiol (E2) 15 ppt 17B-Ethinylestradiol (EE2) 15 ppt Diethylstilbestrol (DES) 5 ppt

1000 2000 3000 4000 5000 6000 7000 2 4 6 8 10 12 14 16

Time (min) Intensity

Estriol Estradiol Estrone Ethinylestradiol Diethylstilbestrol

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9 Environmental Engineering

Automated SPE

AquaAnalysis

  • Parallel on-line sample

prep plus separation and detection system

20 min extraction and instrument run time Reusable HLB cartridges

  • (> 4000 injections)

5 mL to 20 mL sample size

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10 Environmental Engineering

Automated SPE Method

Approxim ate Minim um Detection Lim its ( MDLs) Estrone (E1) 2.5 ppt Estriol (E3) 5 ppt Estradiol (E2) 10 ppt 17B-Ethinylestradiol (EE2) 10 ppt Diethylstilbestrol (DES) 5 ppt

10000 20000 30000 40000 50000 60000 70000 80000 2 4 6 8 10 12 14 16

Time (min) Intensity

Estriol Estradiol Estrone Ethinylestradiol Diethylstilbestrol

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11 Environmental Engineering

Cost Comparison

Capital Costs

  • Instrument Costs

Operations and Maintenance Costs

  • Labor
  • Consumables
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12 Environmental Engineering

Cost Comparison – Capital Costs

Capital Costs Total I nstrum ent Costs Annualized I nstrum ent Costs AquaAnalysis - Automated $349,000 $47,000 Alliance/ Micro – Manual $281,000 $38,000

n = 10 yrs i = 5.5 %

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13 Environmental Engineering

Cost Comparison – Operations & Maintenance

O&M Costs per Sam ple Extraction Colum ns Analyst Tim e I nstrum ent Tim e AquaAnalysis – Automated $0.084 5 min 15 min Alliance/ Micro – Manual $5.30 20 min 16 min

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14 Environmental Engineering

Method Comparison

Manual SPE Method

  • Labor intensive extraction method (8 hours for

24 samples)

  • MDLs of 15 ppt or lower

AquaAnalysis

  • Faster turn-around on samples
  • MDLs of 10 ppt or lower
  • Potential for much lower MDLs with automated

cartridge loading

  • Automated with ability to run over night
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15 Environmental Engineering

Discussion on AquaAnalysis

Contribution to Environmental Engineering

  • Decreases error with all-in-one unit
  • Increases efficiency in sample preparation
  • Eliminates need for large sample volumes
  • Comparable cost to manual extraction with

lower O&M costs

  • Potentially lower MDLs
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16 Environmental Engineering

Special Thanks

Claude Mallet Brad Barrett Chris Shevlin Waters Corporation

FP916940

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17 Environmental Engineering

Questions?