Determination of cyanogenic glycoside linamarin in cassava flour using liquid chromatography-tandem mass spectrometry

Abstract

A specific and reliable method was developed for determining the presence of linamarin, a cyanogenic glucoside in cassava flour and cassava starch, using liquid chromatography-electrospray ionization tandem mass spectrometry. Linamarin was extracted with acetonitrile and then purified by solid-phase clean-up using an NH₂ cartridge column. Isocratic HPLC was used to introduce samples for electrospray negative ionization tandem mass spectrometry. The multiple reaction monitoring (MRM) was performed using a characteristic fragmentation (m/z 246.1→ m/z 161.0) for linamarin. Calibration with a standard solution was linear over a working range of 0.001-0.1 ppm (r²=0.995-0.999), which is equivalent to 0.18-18 μg/g in food samples. The mean recovery of linamarin from cassava flour was approximately 92-100%. The detection limits of the proposed method of linamarin in cassava flour and tapioca samples were 0.75 μg/g and 0.84 μg/g, respectively.