Speciation analysis of organoarsenic species in marine samples: method optimization using fractional factorial design and method validation

• DOI: 10.1007/s00216-021-03341-4
• Publication Date: 2021-05-15T04:02:39Z
• Authors: Jojo Tibon; Marta Silva; Jens J. Sloth; Heidi Amlund; Veronika Sele
• Keywords: Arsenobetaine; Certified reference materials; Fractional factorial design; Genetic algorithm; Sample Preparation; Central composite design

Abstract Organoarsenic species in marine matrices have been studied for many years but knowledge gaps still exist. Most literature focuses on monitoring of arsenic (As) using previously published methods based anion- and cation-exchange high-performance liquid chromatography-inductively coupled plasma mass spectrometry (HPLC-ICP-MS). These studies are often limited to few As and/or only specific method performance characteristics described. certified reference materials (CRMs) arsenobetaine (AB) dimethylarsinate (DMA), making it difficult evaluate the accuracy analytical other organoarsenic species. To address these gaps, main objective this work was develop validate a speciation analysis broad range matrices. Optimum extraction conditions were identified through 2 7–3 fractional factorial design blue mussel as test sample. The effects sample weight, type volume solution, addition H O time temperature, use ultrasonication investigated. highest recoveries obtained by 0.2 g 5 mL aqueous methanol (MeOH:H O, 50% v/v) extractant, carried out at 90 °C 30 min, without ultrasonication. Anion- HPLC-ICP-MS settings subsequently optimized. detected total 33 known unknown within run 23 20 min anion-exchange, respectively. A single-laboratory validation conducted several CRMs: BCR 627 (tuna fish tissue), ERM-CE278k (mussel DORM-4 (fish protein), DOLT-5 (dogfish liver), SQID-1 (cuttlefish), TORT-3 (lobster hepatopancreas), CRM 7405-b (hijiki seaweed). Method evaluated selectivity, limits detection quantification, linearity, trueness, precision, measurement uncertainty. This proposes an procedure which allowed satisfactory quantification with low solvent energy consumption, supporting “Green Chemistry” principles. study also presents new set data, including methylated arsenosugars, recently issued CRMs, will be valuable future As. is first report different CRMs. Graphical abstract