Quantification of Oxidized and Unsaturated Bile Alcohols in Sea Lamprey Tissues by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

Ke Li; Anne M Scott; Yu-Wen Chung-Davidson; Ugo Bussy; Trinkal Patel; Zoe E Middleton; Weiming Li

doi:10.3390/molecules21091119

Quantification of Oxidized and Unsaturated Bile Alcohols in Sea Lamprey Tissues by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry

Molecules. 2016 Aug 24;21(9):1119. doi: 10.3390/molecules21091119.

Authors

Ke Li¹, Anne M Scott², Yu-Wen Chung-Davidson³, Ugo Bussy⁴, Trinkal Patel⁵, Zoe E Middleton⁶, Weiming Li⁷

Affiliations

¹ Department of Fisheries and Wildlife, Michigan State University, East Lansing, MI 48824, USA. like4@msu.edu.
² Department of Fisheries and Wildlife, Michigan State University, East Lansing, MI 48824, USA. scottan7@msu.edu.
³ Department of Fisheries and Wildlife, Michigan State University, East Lansing, MI 48824, USA. chungyuw@msu.edu.
⁴ Department of Fisheries and Wildlife, Michigan State University, East Lansing, MI 48824, USA. bussy@msu.edu.
⁵ Department of Fisheries and Wildlife, Michigan State University, East Lansing, MI 48824, USA. pateltrinkal@gmail.com.
⁶ Department of Fisheries and Wildlife, Michigan State University, East Lansing, MI 48824, USA. middle73@msu.edu.
⁷ Department of Fisheries and Wildlife, Michigan State University, East Lansing, MI 48824, USA. liweim@msu.edu.

Abstract

A sensitive and reliable method was developed and validated for the determination of unsaturated bile alcohols in sea lamprey tissues using liquid-liquid extraction and ultra-high performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS). The liver, kidney, and intestine samples were extracted with acetonitrile and defatted by n-hexane. Gradient UHPLC separation was performed using an Acquity BEH C18 column with a mobile phase of water and methanol containing 20 mM triethylamine. Multiple reaction monitoring modes of precursor-product ion transitions for each analyte was used. This method displayed good linearity, with correlation coefficients greater than 0.99, and was validated. Precision and accuracy (RSD %) were in the range of 0.31%-5.28%, while mean recoveries were between 84.3%-96.3%. With this technique, sea lamprey tissue samples were analyzed for unsaturated bile alcohol analytes. This method is practical and particularly suitable for widespread putative pheromone residue analysis.

Keywords: UPLC-MS/MS; fish; metabolites; sulfated bile alcohol.

MeSH terms

Animals
Cholestanols / chemistry*
Cholestanols / metabolism*
Chromatography, High Pressure Liquid
Lampreys / metabolism*
Mass Spectrometry
Oxidation-Reduction

Substances

Cholestanols