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<p>Grayanotoxins are natural toxins in species of <i>Rhododendron</i> and responsible for food poisoning associated with honey. In this method, to effectively assess the food safety of honey, a sensitive solid phase extraction–ultra-performance liquid chromatography–tandem mass spectrometry method (SPE–UPLC–MS/MS) was developed and validated for simultaneous determination of three crucial Grayanotoxins in honey. The Grayanotoxins were extracted from honey samples with 0.1% formic acid aqueous solution, purified using hydrophilic-lipophilic balance (HLB) SPE cartridge, detected in multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI), and quantified with external standard calibration. The developed method exhibited good linearity, average recoveries ranging from 95.5 to 112.1% and relative standard deviations of 2.8 to 12.7% (<i>n</i> = 6). Among 50 commercially available honey samples analyzed, Rhodojaponin III and Grayanotoxin I were detected in a same batch. The developed method proved to be simple, sensitive, and accurate, which will facilitate the risk monitoring of trace Grayanotoxins in honey to safeguard the food safety of honey products.</p>

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Determination of Three Grayanotoxins in Honey by Solid Phase Extraction-Ultra-Performance Liquid Chromatography-Tandem Mass Spectrometry

  • 期刊论文

  • 发表日期：

    2025年8月15日

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  • Chuan Liu,
  • Leijun Yao,
  • Yanqiu Chen,
  • Peiyu Shi,
  • Hao Lin,
  • Yangyang Zhang,
  • Ting Huang,
  • Wenlin Wu,
  • Juan Song,
  • Qin Dai

摘要

Grayanotoxins are natural toxins in species of Rhododendron and responsible for food poisoning associated with honey. In this method, to effectively assess the food safety of honey, a sensitive solid phase extraction–ultra-performance liquid chromatography–tandem mass spectrometry method (SPE–UPLC–MS/MS) was developed and validated for simultaneous determination of three crucial Grayanotoxins in honey. The Grayanotoxins were extracted from honey samples with 0.1% formic acid aqueous solution, purified using hydrophilic-lipophilic balance (HLB) SPE cartridge, detected in multiple reaction monitoring (MRM) mode with positive electrospray ionization (ESI), and quantified with external standard calibration. The developed method exhibited good linearity, average recoveries ranging from 95.5 to 112.1% and relative standard deviations of 2.8 to 12.7% (n = 6). Among 50 commercially available honey samples analyzed, Rhodojaponin III and Grayanotoxin I were detected in a same batch. The developed method proved to be simple, sensitive, and accurate, which will facilitate the risk monitoring of trace Grayanotoxins in honey to safeguard the food safety of honey products.