Microsoft word - an079_120925.doc
Analysis of Hormones in Water by Automated
Solid Phase Extraction
E. Michael Thurman and Imma Ferrer, Center for Environmental Mass Spectrometry,
University of Colorado, Boulder, CO, USA.
Introduction
Hormones are a group of biologically active compounds
that are of concern because of their negative effects in
living organisms, such as fish and aquatic species. These
biologically-active compounds can enter surface waters
from point and non-point sources such as municipal
wastewater treatment plant (WWTP) discharges, industrial
discharges, urban runoff and animal feeding operations.
Therefore, natural and synthetic hormones are usually
detected in waters receiving wastewater discharge.
Recently, the Environmental Protection Agency (EPA)
published a Candidate Contaminant List (CCL3) which
included some of the most important emerging
contaminants in the environment. In this work, the solid-
phase extraction (SPE) for some of the hormones included
in this list was optimized.
Instrumentation
The Horizon Technology SPE-DEX® 4790 Automated Extraction
System, and the Envision® Platform Controller
- SPE-DEX® 4790 Automated Extraction System - Envision® Controller
Evaporation and Derivatization of Extracts:
The methanol extracts were cleaned up on Florisil
columns, and evaporated to dryness under a stream of
- Quatrro-micro-GC/MS/MS using Agilent 6890 GC
The extracts were then derivatized to their
- Column: Rxi XLB 30 m x 0.25 ID, 0.25 µm film
trimethylsilyltrifluoroacetamide according to the
Table 1: Purge Method
Method Summary
Collection, Preparation, and Extraction:
1. Surface water samples were taken from Boulder Creek
(Boulder, CO) upstream and downstream of a WWTP.
2. A spiking mixture containing 8 labeled hormones (D
Table 2: Extraction Method
medroxyprogesterone, D4-mestranol, D3-nandrolone) was used to spike water samples at a concentration of
Soak Time
3. No additives were added to water samples, and no
4. The SPE-DEX 4790 system was purged using a
5. Water samples were extracted using the SPE-DEX
4790 system with the method shown in Table 2.
Horizon Technology, Inc., 45 Northwestern Dr. Salem, NH, 03079 USA
Analysis of Hormones in Water by Automated Solid Phase Extraction
Sample Analysis:
Three surface water samples (upstream, downstream, and
Helium was used as a carrier with a flow rate of 1 milliliter
near a wastewater source) were analyzed with the
per minute (mL/min) with the injection port maintained at
methodology described in this work and several hormones
275°C. The gas chromatograph was programmed on a
were successfully identified. Results are shown in Table 4.
variable temperature gradient from 100°C to 310°C. For
each target compound, the most abundant diagnostic ion in
Conclusions
the full-scan spectrum was selected as a precursor and
appropriate conditions were selected to maximize the signal
The results demonstrated that the SPE-DEX 4790 using
for three precursor-product transitions. The recoveries for
Atlantic C18 disks can effectively extract hormone
all 8 hormones were obtained by comparing the
compounds from 1-L water samples in a fraction of time
chromatographic areas to an external labeled standard. The
(approx. 40 min). This system allows you to use the
other hormones were quantified relative to the isotopic
original sample bottle rinsing it with all of the extraction
dilution standard (IDS) using a quantification procedure
solvents before the final elution step. This rinsing step
that automatically corrects for losses in the reported
ensures that all the compounds are rinsed off the glass and
chemical concentration based on the absolute method
Results
Acknowledgements
The recoveries for the labeled hormone compounds are
Horizon Technology would like to thank E. Michael
presented in Table 3. In general, acceptable recoveries
Thurman and Imma Ferrer of the Center for Environmental
were obtained for the compounds studied. Also, the
Mass Spectrometry at the University of Colorado in
recoveries were very consistent in the three different water
Boulder for their contributions to this Application Note.
matrices studied, showing that the SPE procedure is
reliable and reproducible.
Table 3: Recovery results for the labeled hormones
Recoveries (%)
Surface Water
Surface Water
Canyon Water
Compound
Upstream
Downstream
Table 4: Concentrations for several hormones identified in surface water samples
Recoveries (ng/L)
Surface Water
Surface Water
Canyon Water
Compound
Upstream
Downstream
Horizon Technology, Inc., 45 Northwestern Dr. Salem, NH, 03079 USA
Source: http://www.horizontechinc.com/PDF/03079_9972997/ApplicationsNotes/AN079_12925_Analysis%20of%20Hormones%20in%20Water%20by%20Automated%20Solid%20Phase%20Extraction.pdf
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