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Aims: A rapid and sensitive liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was validated for determination of prohibited cyproheptadine hydrochloride (CP) in dietary supplements.
Methods: CP was extracted by sonication in methanol for 30 min. The chromatography separation of CP took place on C18 column (100 mm x 2.1 mm, 1.8 µm) with gradient mobile phase of both of acetonitrile and water containing 0.1% formic acid. Multiple reaction monitoring (MRM) in the positive mode was used to quantify and confirm CP at m/z 288.2/191.1 and 288.1/96.0, respectively.
Results: The method was validated according to the AOAC requirements. The linearity ranges were found from 0.1 to 50 ng. mL-1 of CP (R2 = 1). The limit of detection and limit of quantification were 1.5 ng/g or ng/mL and 5 ng/g or ng/mL, respectively. The accuracy was within the range from 92 to 99%, with the relative standard deviation (RSD%) of 2.0-5.9%.
Conclusion: The validated parameters have met the requirement of Association of Official Agricultural Chemists (AOAC). This reliable method would be useful for the monitoring of cyproheptadine in dietary supplements.
Chi tiết bài viết
cyproheptadine, dietary supplements, liquid chromatography-mass spectrometry