Cost-Effective and High-Reliability Analytical Approach for Multitoxin Screening in Bivalve Mollusks by Liquid Chromatography Coupled to Tandem Mass Spectrometry

Abstract

A fast, less expensive, analytical approach with high metrologic reliability was developed to assist an official program for 21 marine biotoxins, monitoring in bivalve mollusks. The simultaneous analysis of lipophilic and hydrophilic marine biotoxins was achieved using a sample preparation protocol based on solid–liquid extraction and low-temperature cleanup, followed by liquid chromatography coupled to tandem mass spectrometry. Samples were extracted with acidified methanol/water (90:10), followed by low-temperature cleanup. Chromatographic separation was obtained using a cyano-bonded silica phase. The mobile phase was composed of water and acetonitrile, with both 0.1% formic acid and 2.5 mmol L–1 ammonium formate. Electrospray ionization was used in both negative and positive modes. The single-laboratory validation approach enabled method performance assessment, and the necessary data to design a model for result expression were yielded. With this purpose, a systematic study of errors and uncertainties was performed. This new analytical approach aimed to minimize the use of highly expensive analytical standards, promoting economic viability to be applied by high-throughput routine laboratories. After its implementation on the Brazilian official monitoring program, positive results near the regulatory limits were obtained, demonstrating the fit for purpose of the method as a surveillance tool.

Recent advancements in LC‐MS based analysis of biotoxins: Present and future challenges

“…The method remarkably reduced the analysis time and cost, while successfully assisting in determining the diverse class of toxins simultaneously. A cost-effective LC-MS/MS approach developed by Molognoni et al (2019) could detect 21 marine lipophilic and hydrophilic toxins simultaneously in bivalve molluscs, that followed solid-liquid extraction, and low-temperature clean-up. The study focused on minimizing the application of expensive analytical standards and establishing an economically viable protocol for routine analysis.…”

Avaliação da presença de biotoxinas marinhas em moluscos bivalves na região da Costeira do Ribeirão em Florianópolis, Santa Catarina

“…Vale salientar que o método utilizado para quantificação de biotoxinas marinhas durante o monitoramento é baseado na metodologia de Molognoni et al (2019) [10], sendo a cromatografia líquida acoplada à espectrometria de massas (LC-MS / MS) com ionização por electrospray (ESI) nos modos positivo e negativo a metodologia utilizada para os ensaios de detecção e quantificação de ficotoxinas em moluscos bivalves [10].…”

“…aos azaspirácidos LQ 40 µg/kg;.Incerteza padrão expandida relativa (k = 2,00) na tomada de decisão no LR: equivalentes ao ácido okadaico 30%; equivalentes aos azaspirácidos 24%; equivalentes à yessotoxina 8%; ácido domóico 2% e equivalentes à saxitoxina 24%. Método de análise: MET POA_SLAV/061/0 [10].…”

Synchronous Fe3+-Enhanced Colorimetric and Liquid SERS-Based Detection of Dopamine Using Core–Shell Plasmonic Nanoparticles

“…Many sensing methods have been investigated for DA detection, such as enzyme-linked immunosorbent assay, , chromatographic separation, , fluorescence sensing, , and electrochemical analysis tools. , However, the application of these methods is commonly limited by the requirements of expertise in operation, high cost, and expensive instrumentation. − Recently, plasmonic nanosensor systems have attracted the attention of many researchers owing to their simplicity, rapid detection, and high sensitivity. − In particular, noble metallic nanoparticles (NMPs), especially gold and silver nanoparticles, have been widely investigated in colorimetric and surface-enhanced Raman scattering (SERS) detection methods due to their unique optical and plasmonic properties, which strongly depend on their size, configuration, and interparticle distance. − Gold nanoparticles (AuNPs) possess attractive features such as chemical stability and simple synthetic methods to give high morphological uniformity. Silver nanoparticles (AgNPs) also exhibit practically useful properties to be used as a sensing probe, and they show a higher plasmonic efficiency than AuNPs. − Therefore, we reasoned that Au–Ag core–shell NPs could provide an excellent platform to develop colorimetric sensing systems. ,, …”