A method for the determination of furosine in royal jelly was developed using ultra performance liquid chromatog-raphy-tandem mass spectrometry.The sample was hydrolyzed with 10.6 mol/L hydrochloric acid at 110℃ for 24 h.Subse-quently,the hydrolyzed sample was purified using a C18 solid phase extraction column and eluted with 3 mol/L hydrochloric acid,followed by dilution in a 1∶1 ratio with pure water.Gradient elution was performed using mobile phases consisting of a 2 mM ammonium formate aqueous solution(containing 0.01％formic acid)and a 2 mM ammonium formate methanol so-lution(containing 0.01％formic acid)on a ACQUITY BEH C18 column.Detected in electrospray positive ionization mode with multiple reaction monitoring(MRM)mode and quantified by matrix matching curve external standard method.The re-sults demonstrated that furosine exhibited excellent linearity within the concentration range of 0.001 25-0.075 00 mg/L,with a correlation coefficient(r2)value of 0.997.The limits of detection(LOD)and quantitation(LOQ)were determined to be as low as 17 μg/kg and 50 µg/kg,respectively.Furthermore,the average recovery rates of furosine at levels corresponding to one,two,and ten times LOQ ranged from 105.8％to 1.19.4％,accompanied by relative standard deviations(RSD)ranging from 0.4％to 4.9％(n=6).This method was successfully employed to determine the content of furosine in twenty batches of royal jelly samples which varied between 68.0 μg/kg and 311.5 µg/kg.The method has a low detection limit,high sensitivi-ty,good accuracy,and is suitable for the determination of furosines in royal jelly.
关键词
蜂王浆/糠氨酸/超高效液相色谱-串联质谱法
Key words
Royal jelly/Furosine/Ultra-performance liquid chromatography tandem mass spectrometry
维普
万方数据