超高效液相色谱-串联质谱法检测功能饮料中那非类新型衍生物OA

A method for the identification and quantification of illegally added novel sildenafil derivatives in functional beverages using ultra-performance liquid chromatography-triple quadrupole mass spectrometry(UPLC-MS/MS)was developed and validated.Functional beverage samples were extracted with acetonitrile and analyzed on an Agilent EC-C18 column(100 mm×3.0 mm,2.7 μm)under gradient elution with acetonitrile-0.1%acetic acid aqueous solution at a flow rate of 0.3 mL/min.The column temperature was maintained at 35℃,and the injection volume was 1 μL.Mass spectrometric detection was performed using electrospray ionization in positive mode(ESI+),with quantification conducted in multiple reaction monitoring mode.The results showed that all four target sildenafil derivatives exhibited good linearity within the range of 0.1〜10.0 μg/mL(r＞0.99).Limits of detection were 0.015 to 0.018 μg/mL and limits of quantification were 0.045 to 0.055 μg/mL.The method demonstrated good repeatability(RSD＜4.0%).Analysis of five commercially available functional beverage samples revealed that three contained illegally added sildenafil derivatives,with concentrations ranging from 0.10 to 2.50 μg/mL.The developed UPLC-MS/MS method was shown to be sensitive,and reliable for detecting illegally added sildenafil derivatives in functional beverages,thereby providing strong support for food safety supervision.