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[PMID]: | 29358154 |
[Au] Autor: | Turner AD; Waack J; Lewis A; Edwards C; Lawton L |
[Ad] Endereço: | Centre for Environment, Fisheries and Aquaculture Science, Barrack Road, The Nothe, Weymouth, Dorset DT4 8UB, United Kingdom. Electronic address: andrew.turner@cefas.co.uk. |
[Ti] Título: | Development and single-laboratory validation of a UHPLC-MS/MS method for quantitation of microcystins and nodularin in natural water, cyanobacteria, shellfish and algal supplement tablet powders. |
[So] Source: | J Chromatogr B Analyt Technol Biomed Life Sci;1074-1075:111-123, 2018 Feb 01. | [Is] ISSN: | 1873-376X |
[Cp] País de publicação: | Netherlands |
[La] Idioma: | eng |
[Ab] Resumo: | A simple, rapid UHPLC-MS/MS method has been developed and optimised for the quantitation of microcystins and nodularin in wide variety of sample matrices. Microcystin analogues targeted were MC-LR, MC-RR, MC-LA, MC-LY, MC-LF, LC-LW, MC-YR, MC-WR, [Asp3] MC-LR, [Dha7] MC-LR, MC-HilR and MC-HtyR. Optimisation studies were conducted to develop a simple, quick and efficient extraction protocol without the need for complex pre-analysis concentration procedures, together with a rapid sub 5min chromatographic separation of toxins in shellfish and algal supplement tablet powders, as well as water and cyanobacterial bloom samples. Validation studies were undertaken on each matrix-analyte combination to the full method performance characteristics following international guidelines. The method was found to be specific and linear over the full calibration range. Method sensitivity in terms of limits of detection, quantitation and reporting were found to be significantly improved in comparison to LC-UV methods and applicable to the analysis of each of the four matrices. Overall, acceptable recoveries were determined for each of the matrices studied, with associated precision and within-laboratory reproducibility well within expected guidance limits. Results from the formalised ruggedness analysis of all available cyanotoxins, showed that the method was robust for all parameters investigated. The results presented here show that the optimised LC-MS/MS method for cyanotoxins is fit for the purpose of detection and quantitation of a range of microcystins and nodularin in shellfish, algal supplement tablet powder, water and cyanobacteria. The method provides a valuable early warning tool for the rapid, routine extraction and analysis of natural waters, cyanobacterial blooms, algal powders, food supplements and shellfish tissues, enabling monitoring labs to supplement traditional microscopy techniques and report toxicity results within a short timeframe of sample receipt. The new method, now accredited to ISO17025 standard, is simple, quick, applicable to multiple matrices and is highly suitable for use as a routine, high-throughout, fast turnaround regulatory monitoring tool. |
[Mh] Termos MeSH primário: |
Cromatografia Líquida de Alta Pressão/métodos Cianobactérias/química Suplementos Nutricionais/análise Microcistinas/análise Peptídeos Cíclicos/análise Frutos do Mar/análise
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[Mh] Termos MeSH secundário: |
Animais Produtos Biológicos/análise Produtos Biológicos/química Bivalves Contaminação de Alimentos Limite de Detecção Modelos Lineares Reprodutibilidade dos Testes Comprimidos Espectrometria de Massas em Tandem/métodos Poluentes Químicos da Água/análise
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[Pt] Tipo de publicação: | JOURNAL ARTICLE |
[Nm] Nome de substância:
| 0 (Biological Products); 0 (Microcystins); 0 (Peptides, Cyclic); 0 (Tablets); 0 (Water Pollutants, Chemical); 0979BIK2QU (nodularin) |
[Em] Mês de entrada: | 1803 |
[Cu] Atualização por classe: | 180305 |
[Lr] Data última revisão:
| 180305 |
[Sb] Subgrupo de revista: | IM |
[Da] Data de entrada para processamento: | 180124 |
[St] Status: | MEDLINE |
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