Abstract: Consumer complaints received by the U.S. Food and Drug Administration in August 2010 about raw organic almonds tasting “bitter” opened an investigation into the presence of bitter almonds in the imported product. Bitter almonds (Prunus amygdalus) contain the cyanogenic glucoside amygdalin, which hydrolyzes to produce cyanide. Ultraviolet–visible spectrophotometry was used to detect and quantitate cyanide, and liquid chromatography-mass spectrometry was utilized to detect amygdalin in the submitted samples. Control bitter almonds were found to contain 1.4 mg cyanide/g and an estimated level of 20–25 mg amygdalin/g. The questioned samples contained between 14 and 42 μg cyanide/g and were positive for the presence of amygdalin. Sweet almonds were found to be negative for both compounds, at levels of detection of 4 μg cyanide/g and 200 μg amygdalin/g.