Rapid and reliable steroid hormone profiling in Tursiops truncatus blubber using liquid chromatography tandem mass spectrometry (LC-MS/MS)

Published

June 1, 2017

Author(s)

Ashley S. Boggs-Russell, Tracey B. Schock, Thomas M. Galligan, Wayne E. McFee, Jeanine S. Morey, Lori Schwacke, John R. Kucklick

Abstract

Monitoring of marine mammal steroid hormone status using matrices alternative to blood is desirable due to the ability to remotely collect samples which minimizes stress. However, measurement techniques in alternative matrices such as blubber described to date are limited in scope in the number and types of hormones measured. Therefore, a new method using bead homogenization to QuEChERS (Quick, Easy, Cheap, Effective, Rugged, and Safe) extraction, post extraction cleanup and analysis by liquid chromatography tandem mass spectrometry (LC-MS-MS) was developed and applied to the measurement of hormone suites in bottlenose dolphin blubber collected from dead stranded animals and using remote biopsy of wild-ranging animals. Two separation techniques as well as bead material for homogenization were examined using stranded dolphin blubber samples. The final method consisting of two LC separations and garnet bead homogenization was tested for extraction efficiencies. Steroids were separated using a biphenyl column for reproductive hormones and C18 column for corticosteroids. Three hormones previously noted in the literature to be present in blubber, testosterone, progesterone, and cortisol, were quantified in addition to previously unmeasured androstenedione, 17- hydroxyprogesterone, 11-deoxycortisol, 11-deoxycorticosterone, and cortisone (previously undetected in blubber) in a single sample (0.4 g). Extraction efficiencies of all hormones from blubber ranged from 81 % and 112 % and all RSDs were comparable to those reported using immunoassay methods (< 15 %). The method was sensitive enough to measure baseline hormone concentrations in remote biopsied blubber samples. Through this method, increased coverage of steroid hormone pathways from a single remotely collected sam

Citation

Analytical and Bioanalytical Chemistry

Pub Type

Journals

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Keywords

liquid chromatography, mass spectrometry, environmental, steroid hormones, marine mammal

Citation

Boggs-Russell, A. , Schock, T. , Galligan, T. , McFee, W. , Morey, J. , Schwacke, L. and Kucklick, J. (2017), Rapid and reliable steroid hormone profiling in Tursiops truncatus blubber using liquid chromatography tandem mass spectrometry (LC-MS/MS), Analytical and Bioanalytical Chemistry, [online], https://tsapps.nist.gov/publication/get_pdf.cfm?pub_id=922670 (Accessed April 25, 2026)

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