Determination of Grayanotoxin I and Grayanotoxin III in mad honey from Nepal using liquid chromatography-tandem mass spectrometry
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Grayanotoxin-contaminated honey exhibits toxicity. In this study, a reliable and sensitive liquidchromatography– tandem-mass-spectrometric method (LC–MS/MS) was developed and validated for the quantitation of grayanotoxin I and grayanotoxin III in honey. The grayanotoxins were extracted from honey via solid phase extraction and separated on a biphenyl column with a mobile phase consisting of 0.5 % acetic acid in water and methanol. Mass spectrometric detection was performed in the multiple-reaction monitoring mode with positive electrospray ionization. The calibration curve covered the range 0.25 to 100 μg/g. The intra- and interday deviations were less than 10.6 %, and the accuracy was between 94.3 and 114.0 %. The validated method was successfully applied to the determination of grayanotoxins in mad honey from Nepal. The concentrations of grayanotoxin I and grayanotoxin III in 33 out of 60 mad honey samples were 0.75 – 64.86 μg/g and 0.25 – 63.99 μg/g, respectively. The method established herein would help in preventing and confirming grayanotoxin poisoning.
Abstract
Grayanotoxin-contaminated honey exhibits toxicity. In this study, a reliable and sensitive liquidchromatography– tandem-mass-spectrometric method (LC–MS/MS) was developed and validated for the quantitation of grayanotoxin I and grayanotoxin III in honey. The grayanotoxins were extracted from honey via solid phase extraction and separated on a biphenyl column with a mobile phase consisting of 0.5 % acetic acid in water and methanol. Mass spectrometric detection was performed in the multiple-reaction monitoring mode with positive electrospray ionization. The calibration curve covered the range 0.25 to 100 μg/g. The intra- and interday deviations were less than 10.6 %, and the accuracy was between 94.3 and 114.0 %. The validated method was successfully applied to the determination of grayanotoxins in mad honey from Nepal. The concentrations of grayanotoxin I and grayanotoxin III in 33 out of 60 mad honey samples were 0.75 – 64.86 μg/g and 0.25 – 63.99 μg/g, respectively. The method established herein would help in preventing and confirming grayanotoxin poisoning.
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