Validation of a gas chromatography–mass spectrometry method for the determination of pg/ml levels of 17β-estradiol and 17β-trenbolone in bovine serum

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• 作者：Fedeniuk ; Rick W. ; Boison ; Joe O. ; MacNeil ; James D.
• 关键词：17&#946 ; -Estradiol ; 17&#946 ; -Trenbolone
• 刊名：Journal of Chromatography B, Analytical Technologies in the Biomedical and Life Sciences
• 出版年：2004
• 出版时间：April 5, 2004
• 年：2004
• 卷：802
• 期：2
• 页码：307-315
• 全文大小：148 K

文摘

A method for the quantitation of pg/ml levels of 17β-estradiol and 17β-trenbolone in bovine serum by gas chromatography/electron-capture mass spectrometry has been developed and validated. Using the area ratios of the integrated molecular-ion peaks of the analytes to their corresponding deuterated internal standards, [2,4,16,16-²H₄] 17β-estradiol (17β-estradiol-d₄) and [16,16-²H₂] 17β-trenbolone (17β-trenbolone-d₂), and non-weighted linear regression, two calibration curves per analyte; 5–50 and 50–500pg/ml for 17β-estradiol in sera, and 25–250 and 250–2500pg/ml for 17β-trenbolone in sera, respectively, were constructed. Splitless injection of 200fg 17β-estradiol and 1000fg 17β-trenbolone could be detected and quantified. Tested batches of control bovine sera did not exhibit interference for 17β-trenbolone, and showed expected background presence of endogenous 17β-estradiol. Intra-day residual errors did not exceed 20 % , and regression correlations were greater than 0.99. Intra-day precision data was similar to inter-day precision data. Using this method, 16 samples can be processed within one working day.