High-sensitivity determination of estrogens in fish plasma using chemical derivatization upstream UHPLC-MSMS

被引:15
作者
Bussy, Ugo [1 ]
Chung-Davidson, Yu -Wen [1 ]
Buchinger, Tyler J. [1 ]
Li, Ke [1 ]
Li, Weiming [1 ]
机构
[1] Michigan State Univ, Dept Fisheries & Wildlife, Room 13 Nat Resources Bldg 480 Wilson Rd, E Lansing, MI 48824 USA
关键词
Steroids; El; E2; E3; LC-MSMS; TANDEM MASS-SPECTROMETRY; ATMOSPHERIC-PRESSURE PHOTOIONIZATION; PERFORMANCE LIQUID-CHROMATOGRAPHY; ZEBRAFISH DANIO-RERIO; ELECTROSPRAY-IONIZATION; LC-MS/MS; HUMAN SERUM; ESTRADIOL; STEROIDS; REAGENT;
D O I
10.1016/j.steroids.2017.04.003
中图分类号
Q5 [生物化学]; Q7 [分子生物学];
学科分类号
071010 ; 081704 ;
摘要
This article describes the development and validation of a sensitive LC-MSMS method for determination of estrogen in fish plasma. Dansyl chloride derivatization of the phenol functional group in estrogen was used to enhance the response to atmospheric pressure ionization leading to improve the sensitivity. Individual C-13 internal standards were selected after comparison with deuterated standards. Liquid-liquid extraction (ethyl acetate or methyl tert-butyl ether) and protein precipitation (acetonitrile, methanol or acetone) were compared for the extraction and clean-up of estrogens from fish plasma. Ethyl acetate was selected as the best alternative with recovery ranging from 61 to 96% and matrix effect ranging from 88 to 106%. Limits of quantification ranged from 0.5 to 1 pg/mL showing a gain in sensitivity of 10,000 times over electrospray ionization of underivatized estrogens. Accuracy and precision were validated over three consecutive days and the method was applied to measure estrogen in sea lamprey (Petromyzon marinus) and lake trout (Salvelinus namaycush) plasma. Estrone and estriol were detected in fish below 1 ng/mL in plasma, justifying the need of a highly sensitive LC-MSMS quantification method.
引用
收藏
页码:13 / 19
页数:7
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