Determination of methyltestosterone in Tilapia by UPLC-MS/MS
In this study,a ultra performance liquid chromatography-tandem mass spectrometry method for the deter-mination of methyltestosterone in tilapia was optimized and established.Tilapia samples were homogenized,extracted by acetonitrile solution containing 1.0％formic acid,purified by QuEChERS,concentrated by nitrogen blowing in water bath,and dissolved in mobile phase.The sample was separated on a BEH C18 column and eluted with a gradient elution of aqueous solution containing 0.1％formic acid and methanol as mobile phase,using ESI positive ion multi-ple reaction monitoring mode in UPLC-MS/MS,and quantitative analysis was used with internal standard method.The results showed that methyltestosterone had a good linear relationship within the linear range.The correlation coef-ficient of the standard curve was 0.999 5.The detection limit was 0.30 μg/kg and the quantitative limit was 1.0 µg/kg.At the different spiked levels(n=6)in tilapia substrate,the average recoveries were 98.3％to 103.0％and the relative standard deviation was 4.2％to 8.8％.The optimized method has high sensitivity,good accuracy,simple and rapid pre-treatment process,which is suitable for the detection of methyltestosterone residues in tilapia.[Chinese Fishery Quality and Standards,2024,14(1):27-34]
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