Rapid Analysis of Steroid Hormone Residues in Fish Flesh by High Performance Liquid Chromatography-tandem Mass Spectrometry
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Abstract:
A rapid and efficient high performance liquid chromatography-tandem mass spectrometry method was established for the analysis of steroid hormones in fish flesh. The conditions for chromatographic separation and triple-quadrupole mass spectrometry detection were optimized. Baseline separation was achieved for most of the substances within 20 min using a Hypersil GOLD C18 column (150 mm×2.1 mm, i.d. 5 μm) and gradient elution with methanol-water (containing 0.1% formic acid, V/V, %). Most compounds were baseline separated in 20 min. Electrospray ionization in positive ion mode with selective ion pairing, along with the retention time and characteristic ion pairs of the target compound, was used for qualitative and quantitative analyses of 16 steroid hormones. The results showed that all compounds had a good linear range of 0.10~3000.00 ng/mL, with correlation coefficient R greater than 0.9987 and limit of detection in range of 0.05~5.00 ng/mL. Fish flesh was ground into powder in liquid nitrogen, and the latter was purified by solid phase extraction. The hydrocortisone drug residue in fish powder was 48.00 ng/g. The recoveries of 16 steroid hormones were in range of 82.84%~115.10%, with the RSD values lower than 9.30%. This method had high separation power and high sensitivity, and is suitable for simultaneous determination of steroid hormones in aquatic products.
