Reversed-phase/weak anion exchange magnetic mesoporous microspheres for removal of matrix effects in lipophilic marine biotoxins analysis by ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry

• Published in: Food chemistry 2019-10, Vol.294, p.104-111
• Main Authors: Xu, Fei, Liu, Feng, Wang, Chaozhan, Wei, Yinmao
• Format: Article
• Language: English
• Subjects: Chromatography, High Pressure Liquid; Ferrosoferric Oxide - chemistry; Limit of Detection; Lipophilic marine biotoxins; Magnetic solid-phase extraction; Magnetics; Marine Toxins - analysis; Marine Toxins - isolation & purification; Microspheres; Mix-mode mesoporous magnetic adsorbent; Okadaic Acid - analysis; Okadaic Acid - isolation & purification; Porosity; Shellfish - analysis; Silicon Dioxide - chemistry; Solid Phase Extraction; Spiro Compounds - analysis; Spiro Compounds - isolation & purification; Tandem Mass Spectrometry; Ultrahigh-performance liquid chromatography coupled to tandem mass spectrometry
• ISSN: 0308-8146; 1873-7072
• DOI: 10.1016/j.foodchem.2019.05.031

•Mix-mode magnetic mesoporous SiO2 was applied for enrichment of lipophilic marine biotoxins.•The adsorbent showed good selectivity and high adsorption capacity toward target analytes.•Matrix effects with shellfish were reduced effectively using magnetic solid-phase extraction.•Six marine biotoxins in shellfish were quantified simultaneously using LC-MS/MS. Magnetic solid-phase extraction (MSPE), using a new reversed-phase/weak anion exchange mix-mode mesoporous magnetic SiO2 adsorbent, was assessed as an approach for reducing matrix effects in the analysis of six lipophilic marine biotoxins in shellfish using ultrahigh-performance liquid chromatography tandem mass spectrometry (UPLC-MS/MS). The adsorbent showed greater adsorption capacity and selectivity for the analytes and, thus, the MSPE microspheres reduced the matrix effects significantly in the subsequent analysis. In the UPLC-MS/MS analysis, precursor and product ions of the analytes were monitored quantitatively and qualitatively using multiple reaction monitoring and product ion confirmation modes. The proposed method exhibited a linear correlation of 0.9980–0.9991 in the working range for azaspiracids (2.0–200.0 ng/mL) and okadaic acid and its derivatives dinophysistoxins (4.0–200.0 ng/mL) with satisfactory recoveries (82.8–118.6%, RSD