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<p>Arsenic is a ubiquitous environmental contaminant, and its toxicological impact is highly dependent on its speciation. In marine edible algae, increasingly consumed for their nutritional value, arsenosugars (As-Sugars) constitute the major arsenic forms. Despite their generally low toxicity, their uncertain long-term effects make accurate identification essential. We developed an analytical workflow combining ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS). Both Q-Orbitrap and IMS-Q-TOF systems were employed, operating in positive and negative electrospray ionization (ESI) modes. Using a zwitterionic hydrophilic interaction liquid chromatography (HILIC-Z) column, we achieved effective separation of the target compounds and subsequently performed detailed HRMS and MS/MS analyses. This approach enabled the structural annotation of four key As-Sugars (Gly-Sug, PO<sub>4</sub>-Sug, SO<sub>3</sub>-Sug, and SO<sub>4</sub>-Sug) on the basis of accurate mass measurements and diagnostic fragmentation patterns. Notably, we report for the first time the collision cross-section (CCS) values of these As-Sugars, providing an additional orthogonal parameter that strengthens their confirmation.</p> Graphical abstract <p></p>

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Comprehensive profiling of arsenosugars in algae using UHPLC-HRMS and UHPLC-IMS-Q-TOF

  • 期刊论文

  • 出版模式：

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  • 发表日期：

    2026年3月27日

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  • Alba Morales-Rodríguez,
  • Àngels Sahuquillo,
  • José Fermín López-Sánchez,
  • Dolores Barrón,
  • Encarnación Moyano

摘要

Arsenic is a ubiquitous environmental contaminant, and its toxicological impact is highly dependent on its speciation. In marine edible algae, increasingly consumed for their nutritional value, arsenosugars (As-Sugars) constitute the major arsenic forms. Despite their generally low toxicity, their uncertain long-term effects make accurate identification essential. We developed an analytical workflow combining ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS). Both Q-Orbitrap and IMS-Q-TOF systems were employed, operating in positive and negative electrospray ionization (ESI) modes. Using a zwitterionic hydrophilic interaction liquid chromatography (HILIC-Z) column, we achieved effective separation of the target compounds and subsequently performed detailed HRMS and MS/MS analyses. This approach enabled the structural annotation of four key As-Sugars (Gly-Sug, PO4-Sug, SO3-Sug, and SO4-Sug) on the basis of accurate mass measurements and diagnostic fragmentation patterns. Notably, we report for the first time the collision cross-section (CCS) values of these As-Sugars, providing an additional orthogonal parameter that strengthens their confirmation.

Graphical abstract