Detection and quantification of metastable photoproducts of trenbolone and altrenogest using liquid chromatography–tandem mass spectrometry

Philip T Kenyon; Haoqi Zhao; Xingjian Yang; Christopher Wu; David M Cwiertny; Edward P Kolodziej

doi:10.1016/j.chroma.2019.06.030

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Detection and quantification of metastable photoproducts of trenbolone and altrenogest using liquid chromatography–tandem mass spectrometry

Journal article

Open access

Peer reviewed

Detection and quantification of metastable photoproducts of trenbolone and altrenogest using liquid chromatography–tandem mass spectrometry

Philip T Kenyon, Haoqi Zhao, Xingjian Yang, Christopher Wu, David M Cwiertny and Edward P Kolodziej

Journal of Chromatography A, Vol.1603, pp.150-159

10/11/2019

DOI: 10.1016/j.chroma.2019.06.030

PMID: 31227361

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Abstract

•Unstable photoproducts of trenbolone and altrenogest were quantified via LC–MS/MS.•Photoproducts were generated onsite with solar simulator.•Cold, neutral conditions, fast processing, and [M + Na]+ control improve performance.•SPE extracts of photoproducts are stable for up to a month.•Sample acidification can be used to quantify photoproducts indirectly. Here, we developed a novel and sensitive method for the detection and quantification of metastable trenbolone and altrenogest photoproducts in agricultural receiving waters based on solid phase extraction (SPE) and liquid chromatography-tandem mass spectrometry (LC–MS/MS). Primary method analytes were seven cycloaddition or photohydration transformation products of 17α-trenbolone (17α-TBOH), 17β-trenbolone (17β-TBOH), trendione (TBO), and altrenogest (ALT), which are key contributors to the fate and environmental risks of these steroidal pharmaceuticals. Because commercial analytical standards are not available, reference standards for photoproducts were generated from trenbolone or ALT with a solar simulator (˜6 h, >10 half-lives). Efficient detection of metastable photoproducts required cold and pH neutral conditions, rapid sample processing, minimal sample storage, and consideration of cationic artifacts. Method detection limits (MDLs) were 0.034-0.40 ng L−1 for parent compounds and 0.16–2.1 ng L−1 for photoproducts, sufficient for their detection in agroecosystems. Matrix suppression was observed and corrected by internal standards, and relative recovery rates were near 100% for all analytes except for 12-OH-17α-TBOH (˜75% recovery). Intra-day variation was <20% and inter-day variation <25% for all the analytes. The developed method is capable of the analysis of trenbolone, altrenogest, and their key bioactive photoproducts in agricultural receiving waters.

Altrenogest

LC–MS/MS

Metastable

Photoproduct

Trenbolone

Details

Title: Subtitle: Detection and quantification of metastable photoproducts of trenbolone and altrenogest using liquid chromatography–tandem mass spectrometry
Creators: Philip T Kenyon - University of Washington
Haoqi Zhao - University of Washington
Xingjian Yang - South China University of Technology
Christopher Wu - University of Washington
David M Cwiertny - University of Iowa
Edward P Kolodziej - University of Washington
Resource Type: Journal article
Publication Details: Journal of Chromatography A, Vol.1603, pp.150-159
Publisher: Elsevier B.V
DOI: 10.1016/j.chroma.2019.06.030
PMID: 31227361
ISSN: 0021-9673
eISSN: 1873-3778
Grant note: DOI: 10.13039/100000199, name: U.S. Department of Agriculture
Language: English
Date published: 10/11/2019
Academic Unit: Center for Health Effects of Environmental Contamination; Civil and Environmental Engineering; Public Policy Center (Archive); Chemistry; Chemical and Biochemical Engineering
Record Identifier: 9984197240602771

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