Rapid Determination of Illegally Added 25 Hormones in Oral by Ultra Performance Liquid Chromatography-Tandem Mass Spectrometry[J]. 2014,33(6):635-641.DOI:
A sensitive ultra performance liquid chromatography-tandem mass spectrometric(UPLC-MS/MS) method was developed for the simultaneous determination of 9 progesterones,7 androgens,7 glucocorticoids,2 estrogens in anti-aging oral samples.The analytes were stepwise extracted with acetonitrile containing 1% acetic acid and methanol,the extract was concentrated to dryness,redissolved in methanol-water(1∶1).25 hormones were gradient separated on a Shim-pack XR-ODS Ⅱ column,and analyzed by electrospray ionization under positive ion mode with matrix standard curve.As a result,the calibration curves for all target compounds were linear in the range of 0.5-50 μg/L with correlation coefficients larger than 0.99.The limits of detection(LOD) ranged from 0.029 μg/kg to 0.147 μg/kg and the limits of quantitation(LOQ) ranged from 0.099 μg/kg to 0.492 μg/kg.The average recoveries of 25 compounds at spiked levels of 0.5,1.0,5.0 μg/kg were in the range of 73.3%-122.2% with relative standard deviations(RSD) of 5.1%-14.9%.The method is simple,rapid and accurate,and is suitable for the rapid determination of hormones in anti-aging function foods.
关键词
口服液激素超高效液相色谱-串联质谱法(UPLC-MS/MS)
Keywords
oralhormoneultra performance liquid chromatography-tandem mass spectrometry(UPLC-MS/MS)