Advanced

Analysis of selected natural and synthetic hormones by LC-MS-MS using the US EPA method 1694

Sapozhnikova, Yelena; Hedgespeth, Melanie LU ; Wirth, Edward and Fulton, Michael (2011) In Analytical Methods 3. p.1079-1086
Abstract
The US EPA Method 1694 (which is specific to the analysis of pharmaceuticals and personal care products) was evaluated for analysis of selected hormones: 17a- and 17b-estradiol, estriol, estrone, 17a-ethynylestradiol, diethylstilbestrol, equilin, equilenin, testosterone, progesterone and norgestrel in filtered sewage influent/effluent and seawater. The extraction of hormones from fortified water matrices with HLB Oasis solid phase extraction cartridges resulted in good recovery efficiencies: 86–113% for seawater and 80–114% for sewage samples with a relative standard deviation of 6–16% (seawater) and 7–14% (wastewater). Natural and synthetic estrogens (17a- and 17b-estradiol, estriol, estrone, 17a-ethynylestradiol, diethylstilbestrol,... (More)
The US EPA Method 1694 (which is specific to the analysis of pharmaceuticals and personal care products) was evaluated for analysis of selected hormones: 17a- and 17b-estradiol, estriol, estrone, 17a-ethynylestradiol, diethylstilbestrol, equilin, equilenin, testosterone, progesterone and norgestrel in filtered sewage influent/effluent and seawater. The extraction of hormones from fortified water matrices with HLB Oasis solid phase extraction cartridges resulted in good recovery efficiencies: 86–113% for seawater and 80–114% for sewage samples with a relative standard deviation of 6–16% (seawater) and 7–14% (wastewater). Natural and synthetic estrogens (17a- and 17b-estradiol, estriol, estrone, 17a-ethynylestradiol, diethylstilbestrol, equilin, equilenin) were separated with a Gemini-NX C18 (Phenomenex, Inc.) column and detected by Liquid Chromatography Tandem Mass Spectrometry (LC-MS-MS) in negative ElectroSpray Ionization (ESI) multiple reaction monitoring (MRM) mode. Three other hormones (testosterone, progesterone and norgestrel) were separated using an Xterra MS C18 (Waters Corp.) column along with the Group I compounds of the EPA Method 1694 and detected by MS–MS in ESI positive mode. Most compounds were quantified by isotope dilution with matched labeled internal standards. The method was applied to the analysis of effluent and influent from wastewater treatment facilities in South Carolina, USA, and surface seawater samples from Charleston Harbor, South Carolina. Only estrone was detected in surface seawater at a concentration of 0.5 ng/L, which was below the method reporting limit of 1 ng/L. Estriol, estrone and testosterone were found in influent samples at 155–179 ng/L, 27–28 ng/L and 41–49 ng/L, respectively. The estrone concentration was 24 ng/L in an effluent sample from one of the treatment plants. This study demonstrates that the US EPA Method 1694 can be successfully used for the analysis of natural and synthetic hormones along with the pharmaceuticals and personal care products (PPCPs) currently listed in the method. (Less)
Please use this url to cite or link to this publication:
author
publishing date
type
Contribution to journal
publication status
published
subject
in
Analytical Methods
volume
3
pages
1079 - 1086
publisher
Royal Society of Chemistry
external identifiers
  • Scopus:79959754853
ISSN
1759-9660
DOI
10.1039/C0AY00748J
language
English
LU publication?
no
id
fabb3a82-efe5-4f54-80f8-c212413b724c (old id 4359188)
date added to LUP
2014-03-13 16:00:29
date last changed
2017-01-01 08:17:57
@article{fabb3a82-efe5-4f54-80f8-c212413b724c,
  abstract     = {The US EPA Method 1694 (which is specific to the analysis of pharmaceuticals and personal care products) was evaluated for analysis of selected hormones: 17a- and 17b-estradiol, estriol, estrone, 17a-ethynylestradiol, diethylstilbestrol, equilin, equilenin, testosterone, progesterone and norgestrel in filtered sewage influent/effluent and seawater. The extraction of hormones from fortified water matrices with HLB Oasis solid phase extraction cartridges resulted in good recovery efficiencies: 86–113% for seawater and 80–114% for sewage samples with a relative standard deviation of 6–16% (seawater) and 7–14% (wastewater). Natural and synthetic estrogens (17a- and 17b-estradiol, estriol, estrone, 17a-ethynylestradiol, diethylstilbestrol, equilin, equilenin) were separated with a Gemini-NX C18 (Phenomenex, Inc.) column and detected by Liquid Chromatography Tandem Mass Spectrometry (LC-MS-MS) in negative ElectroSpray Ionization (ESI) multiple reaction monitoring (MRM) mode. Three other hormones (testosterone, progesterone and norgestrel) were separated using an Xterra MS C18 (Waters Corp.) column along with the Group I compounds of the EPA Method 1694 and detected by MS–MS in ESI positive mode. Most compounds were quantified by isotope dilution with matched labeled internal standards. The method was applied to the analysis of effluent and influent from wastewater treatment facilities in South Carolina, USA, and surface seawater samples from Charleston Harbor, South Carolina. Only estrone was detected in surface seawater at a concentration of 0.5 ng/L, which was below the method reporting limit of 1 ng/L. Estriol, estrone and testosterone were found in influent samples at 155–179 ng/L, 27–28 ng/L and 41–49 ng/L, respectively. The estrone concentration was 24 ng/L in an effluent sample from one of the treatment plants. This study demonstrates that the US EPA Method 1694 can be successfully used for the analysis of natural and synthetic hormones along with the pharmaceuticals and personal care products (PPCPs) currently listed in the method.},
  author       = {Sapozhnikova, Yelena and Hedgespeth, Melanie and Wirth, Edward and Fulton, Michael},
  issn         = {1759-9660},
  language     = {eng},
  pages        = {1079--1086},
  publisher    = {Royal Society of Chemistry},
  series       = {Analytical Methods},
  title        = {Analysis of selected natural and synthetic hormones by LC-MS-MS using the US EPA method 1694},
  url          = {http://dx.doi.org/10.1039/C0AY00748J},
  volume       = {3},
  year         = {2011},
}