Objective To establish a method for the simultaneous determination of biotin in special dietary foods by ultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS).Methods The samples were added internal standard substance and warm water of 40℃,and were ultrasonically extracted after oscillation and mixing,then cooled to room temperature.The pH values of the samples were then adjusted to 1.6±0.2 with perchloric acid.After centrifugation,the pH values of the supernatant were adjusted to 4.5±0.2 by sodium hydroxide.After being centrifuged again,the supernatant was filtered by 0.22 μm filter membrane,then was separated with Kinetex RR-C18(100 mm×2.1 mm,2.6 μm)column,using 0.1%formic acid aqueous solution-acetonitrile as mobile phase.The quantitative analysis was performed through internal standard method.Results The biotin had good linear relationship in the range of 1-50 ng/ml(r>0.999).The limit of detection was 0.003 μg/g,and the limit of quantitation was 0.01 μg/g.The content of biotin in sample extract solution was stable within 10 h,and the RSD was 5.87%.The average recoveries at the spiked levels of 5,15,30 ng/ml were 90.7%-116.9%,with RSDs of 1.71%-4.42%(n=6).Conclusion This method has fast detection speed,high sensitivity and good repeatability,and is suitable for rapid detection and confirmatory analysis of biotin in special dietary foods.
关键词
生物素/特殊膳食食品/超高效液相串联三重四极杆质谱法
Key words
biotin/special dietary food/ultra performance liquid chromatography-tandem mass spectrometry
维普
万方数据