| Title: | Multiplex quantification of lamprey specific bile acid derivatives in environmental water using UHPLC-MS/MS |
| Author(s): | Li K; Wang H; Brant CO; Ahn S; Li W; |
| Address: | "Department of Fisheries and Wildlife, Michigan State University, East Lansing, MI 48824, United States" |
| Journal Title: | J Chromatogr B Analyt Technol Biomed Life Sci |
| DOI: | 10.1016/j.jchromb.2011.10.039 |
| ISSN/ISBN: | 1873-376X (Electronic) 1570-0232 (Linking) |
| Abstract: | "Larval and adult sea lampreys (Petromyzon marinus) release bile salts and acids into the surrounding aquatic environment. Some of these bile salts and acids, such as petromyzonol sulfate (PZS), 3-keto petromyzonol sulfate (3k PZS), petromyzonamine disulfate (PADS), petromyzosterol disulfate (PSDS), and 3-keto allocholic acid (3k ACA), may function as pheromones. To examine the release and distribution patterns of these metabolites, which this study has termed bile acid derivatives, we developed a novel UHPLC-MS/MS method that was characterized by simple sample preparation, baseline separation, and short analysis time for all studied compounds. These five analytes were separated in 7 min using a reversed-phase C18 column containing 1.7 mum particles and a gradient elution at pH 8.9. Once separated, the analytes were subjected to electrospray ionization-mass spectrometry (negative ion mode) and collision-induced dissociation tandem mass spectrometry (CID-MS/MS) using the multiple reaction monitoring (MRM) mode. Deuterated 3k PZS ([(2)H(5)]3k PZS) was added as the internal standard (IS) to the sample prior to solid phase extraction (SPE). Among the three types of SPE sorbent tested, mixed-mode cation-exchange and reversed-phase sorbent for bases (MAX) and acids (MCX), and reversed-phase C18 sorbent (Sep-pak), the best recoveries (84.1-99.7%) were obtained with MCX cartridges. The calibration curves of all five analytes were linear between 0.15 and 1200 ng/mL, with R(2)>/=0.9997. This method had a precision of relative standard deviation (RSD) /=92.5%. The developed method was successfully used to quantify bile acid derivatives found in streams where lampreys spawn (SD<1.4) and water conditioned with male sea lampreys (SD<4.8). Utilizing this method provides a routine analysis of lamprey bile acid derivatives and may prove useful for sea lamprey population estimates in future studies and applications" |
| Keywords: | "Animals Bile Acids and Salts/*analysis/metabolism Cholestanes/analysis Cholic Acids/analysis Chromatography, High Pressure Liquid/*methods Chromatography, Reverse-Phase Least-Squares Analysis Limit of Detection Male Petromyzon/*metabolism Pyrrolidinones/a;" |
| Notes: | "MedlineLi, Ke Wang, Huiyong Brant, Cory O Ahn, SangChun Li, Weiming eng Research Support, Non-U.S. Gov't Netherlands 2011/11/23 J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Dec 15; 879(32):3879-86. doi: 10.1016/j.jchromb.2011.10.039. Epub 2011 Nov 4" |
