Identifying N-nitrosofenfluramine in a nutrition supplement.
The analytical data for identifying an unknown substance that was found in a nutrition supplement is presented. The unknown substance is purified using thin-layer chromatography and then measured using high-resolution mass spectrometry (HRMS) giving the exact mass from which the structure of the unknown substance was proposed. The procedure for synthesizing N-nitrosofenfluramine from fenfluramine is described. The extracted, synthesized, and standard N-nitrosofenfluramine are compared using HRMS, high-performance liquid chromatography (HPLC)-MS, HPLC-UV, Fourier transform IR spectroscopy, gas chromatography-MS, TLC, and NMR (1H NMR and 13C NMR). All analytical data obtained confirm that the unknown peak in the nutrition supplement is N-nitrosofenfluramine and that the synthetic procedure described can easily provide the N-nitrosofenfluramine reference substance for identification.
Wu
Moutian
M
China Doping Control Center, National Research Institute of Sports Medicine, Beijing, China.
Wang
Jingzhu
J
Wang
Shan
S
Lu
Jianghai
J
Zhang
Yinong
Y
Liu
Xin
X
Zhang
Huyue
H
D002851:Chromatography, High Pressure Liquid; D002855:Chromatography, Thin Layer; D019587:Dietary Supplements / Q000032:analysis*; D004300:Doping in Sports / Q000517:prevention & control; D005277:Fenfluramine / Q000031:analogs & derivatives* / Q000032:analysis* / Q000138:chemical synthesis / Q000737:chemistry; D008401:Gas Chromatography-Mass Spectrometry; D007202:Indicators and Reagents; D009682:Magnetic Resonance Spectroscopy; D013058:Mass Spectrometry; D009747:Nutritional Physiological Phenomena; D021241:Spectrometry, Mass, Electrospray Ionization; D017550:Spectroscopy, Fourier Transform Infrared
D007202:Indicators and Reagents; C493137:nitrosofenfluramine; D005277:Fenfluramine