High-throughput Screening of 13 Digestive Drugs Adulterated Illegally in Biochemical Drugs,Chinese Patent Medicines and Dietary Supplements by Orbitrap High-resolution Mass Spectrometry

KeyWord:digestive drug  illegally adulteration  Orbitrap high resolution mass spectrometry  determination  high-throughput screening

Abstract:

      A method was established for the high-throughput screening of 13 digestive drugs adulterated in biochemical drugs,Chinese patent medicines and dietary supplements by high-performance liquid chromatography-Orbitrap high resolution mass spectrometry(UHPLC-HRMS).Samples were extracted with methanol-water(50¡Ã50£¬by volume),chromatographically separated on a Hypersil Gold C18(2.1 mm¡Á100 mm,3 ¦Ìm) column with acetonitrile-0.1% formic acid as mobile phase by gradient elution.The analysis time for a single injection was merely 10 min.MS detection was performed in positive ion Full MS/dd-MS2 scan mode.Comparing the chromatographic retention time,high resolution primary and secondary mass spectra of the sample with those of the reference substance,it could be judged whether the digestive drug was adulterated into the test samples or not,and the positive samples were quantified.The linear ranges for these 13 digestive drugs were all 8.0-800 ¦Ìg/L with their correlation coefficients(r) no less than 0.998 5.The recoveries were over the range of 94.6%-106.2% with relative standard deviations of 1.2%-2.9%.With the advantages of rapidness,simplicity,high-throughput,good selectivity and high sensitivity,this method was used for the high-throughput screening and determination on 13 kinds of digestive chemicals adulterated in biochemical drugs,Chinese patent medicines and dietary supplements.Five batches of positive samples were found in 38 batches of Chinese patent medicines,and three batches of positive samples were found in 43 batches of dietary supplements.