<p>A validated liquid chromatography–inductively coupled plasma mass spectrometry (LC–ICP–MS) method was developed for procedurally simple and reliable speciation of methylmercury in seafood. Chromatographic separation was achieved using a ZORBAX SB-C18 column under isocratic conditions following a single-step aqueous L-cysteine extraction (1% w/v, 60&#xa0;°C, 120&#xa0;min), providing baseline resolution of methylmercury and inorganic mercury within 4&#xa0;min. Method validation, performed in accordance with AOAC and ICH guidelines, demonstrated excellent linearity (R² = 0.9947), recoveries ranging from 80% to 105%, precision with RSD values within AOAC/ICH acceptance limits (≤ 15%), and good method robustness. The method exhibited high analytical sensitivity, with limits of detection and quantification of 0.26 and 0.78&#xa0;µg/kg, respectively. Applicability was evaluated through the analysis of 100 seafood samples, including finfish, shellfish, cephalopods, and processed products, of which 63 samples contained detectable mercury species. The consistent performance across diverse matrices confirms the suitability of the method for routine application. Compared with microwave- or ultrasound-assisted extraction approaches, the proposed workflow provides a simpler, lower-toxicity, and species-preserving alternative that prioritizes analytical reliability and operational simplicity for routine mercury speciation.</p>

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Assessment of mercury species in edible marine products using advanced LC-ICP-MS technique

  • G Manjushree,
  • A. K Usha,
  • Aadhrika Subrah T,
  • Siva Sankara Reddy Singam

摘要

A validated liquid chromatography–inductively coupled plasma mass spectrometry (LC–ICP–MS) method was developed for procedurally simple and reliable speciation of methylmercury in seafood. Chromatographic separation was achieved using a ZORBAX SB-C18 column under isocratic conditions following a single-step aqueous L-cysteine extraction (1% w/v, 60 °C, 120 min), providing baseline resolution of methylmercury and inorganic mercury within 4 min. Method validation, performed in accordance with AOAC and ICH guidelines, demonstrated excellent linearity (R² = 0.9947), recoveries ranging from 80% to 105%, precision with RSD values within AOAC/ICH acceptance limits (≤ 15%), and good method robustness. The method exhibited high analytical sensitivity, with limits of detection and quantification of 0.26 and 0.78 µg/kg, respectively. Applicability was evaluated through the analysis of 100 seafood samples, including finfish, shellfish, cephalopods, and processed products, of which 63 samples contained detectable mercury species. The consistent performance across diverse matrices confirms the suitability of the method for routine application. Compared with microwave- or ultrasound-assisted extraction approaches, the proposed workflow provides a simpler, lower-toxicity, and species-preserving alternative that prioritizes analytical reliability and operational simplicity for routine mercury speciation.