High-throughput screening and rapid quantification of 60 illegally added chemical drugs in dietary supplements by UPLC-MRM-IDA-EPI
Objective To establish a high-throughput analytical method to monitor and quantify 60 illegally added chemical drugs by UPLC-MRM-IDA-EPI.Methods Samples were analyzed by a Phenomenex kinetex C18(100 mm×3.0 mm,2.6 μm)column with 0.1％formic acid water solution(A)and methanol(B)as the mobile phase with gradient elution at 0.3 mL·min-1.The column temperature was 40 ℃ and the injection volume was 5 μL.The electrospray ionization(ESI)-MS was used in both positive and negative ion mode with MRM-IDA-EPI to establish an EPI database of 60 standard chemical drugs.Suspected compounds were monitored by MRM scan mode and further determined by MRM-IDA-EPI.Results We successfully established an EPI database for each chemical drug and applied the database for compound monitoring and quantification.All the linear calibration curves were obtained with r≥0.99 and the precision of the method was satisfactory with relative standard deviation(RSD)ranging from 0.70％to 7.0％(n=6).The recovery at low,middle,and high concentrations ranged from 60.1％to 115.8％.The limit of detection was at 2.5～1101 ng·g-1.The database used for identification was further verified by analyzing standards in the matrix,and the similarity value("Purity")of each compound ranged from 68 to 95.Totally 30 batches of samples were tested by this method.Nitrazepam,tadalafil and sildenafil were detected in 4 samples.Conclusion The method is efficient and easy to operate for the rapid monitoring of 60 illegally added chemical drugs in dietary supplements.
health foodillegal additionUPLC-MS/MShigh-throughput screening
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