Separation and determination of amygdalin and unnatural neoamygdalin in natural food supplements by HPLC-DAD.

This work is focused on separation and determination of amygdalin and its unnatural form neoamygdalin in natural food supplements. Reversed-phase high-performance liquid chromatography with a high-stability silica-based column with C18 functional group has been used for solving this problem. The effect of the mobile phase composition as well as the column temperature on the separation of the amygdalin epimers has been investigated. Isocratic elution using a mobile phase composed of 0.05% aqueous formic acid and acetonitrile achieved the required separation within 17 min. Under optimum chromatographic conditions, the developed method was validated and was applied for the determination of amygdalin epimers in natural food supplements containing apricot or peach kernels. A simple extraction method using methanol as an extractant supported by an ultrasonic bath was used with recovery in the range of 94.8% to 104.3%. The limit of detection and limit of quantification values for R-amygdalin were 0.13 mg/L and 0.40 mg/L, respectively. The developed method proved to be precise with the intra-day and inter-day relative standard deviation values less than 2.23%.

Colchicine Extract Suicidal Lethal Poisoning Confirmation Using High-Resolution Accurate Mass Spectrometry: A Case Study.

A case of suspected acute and lethal intoxication caused by colchicine has been reported. The woman was hospitalized after her suspicion of suicidal poisoning by a rare autumn crocus (Colchicum autumnale). Suspected colchicine poisoning was confirmed using a novel UHPLC method with a modern reversed-phase stationary phase with a sub 2-micron superficial porous particle size combined with a QTOF mass spectrometer. Sample preparation procedure included the addition of propiverine as internal standard, protein precipitation using methanol and solid phase extraction. High-resolution MS only and targeted MS/MS modes are reported for the qualitative analysis and screening of other potential drugs of abuse in blood samples. All Ion MS mode was used for quantitative determination of colchicine afterward. The concentration of colchicine in the blood sample was approximately 41 ng/mL, and more than 200 µg/mL of the plant extract used for the suicide.