Development and optimization of a method for the determination of Cylindrospermopsin from strains of Aphanizomenon cultures: Intra-laboratory assessment of its accuracy by using validation standards

• Type: Article in International Scientific Journal
• Date: 2012

Authors

Remedios Guzmán-Guillén (Author) Other; Ana I Prieto Ortega (Author) Other; Moreno, I (Author) Other; Gustavo González (Author) Other; Eugenia Soria-Díaz, M (Author) Other; Vitor Vasconcelos (Author) Other; Ana M Cameán (Author) Other

Journal

Title: Talanta

Vol. 100

Pages: 356-363

ISSN: 0039-9140

Publisher: Elsevier

Indexing

ISI Web of Knowledge - 23 Citations

Scopus - 24 Citations

Other information

Authenticus ID: P-002-4E3

DOI: 10.1016/j.talanta.2012.07.087

Abstract (EN): The occurrence of cyanobacterial blooms in aquatic environments is increasing in many regions of the world due to progressive eutrophication of water bodies. Because of the production of toxins such as Cylindrospermopsin (CYN), contamination of water with cyanobacteria is a serious health problem around the world. Therefore it is necessary to develop and validate analytical methods that allow us to quantify CYN in real samples in order to alert the public of this toxin. In this work, an analytical method has been developed an optimized for the determination of CYN from Aphanizomenon ovalisporum cultures. The analytical procedure is based on solvent extraction followed by a purification step with graphitized cartridges and CYN quantification by LC-MS/MS. The extraction and purification steps were optimized using a two-level full factorial design with replications. A suitable and practical procedure for assessing the trueness and precision of the proposed method has been applied by using validation standards. The method has been suitably validated: the regression equation was calculated from standards prepared in extracts from lyophilized M. aeruginosa PCC7820 (r2 >= 0.9999) and the linear range covered is from 5 to 500 mu g CYN/L, equivalent to 0.18-18.00 mu g CYN/g dry weight lyophilized cells. Limits of detection and quantification were 0.04 and 0.15 mu g CYN/g, respectively, the recovery range (%) oscillated between 83 and 94% and intermediate precision (RSD %) values from 5.6 to 11.0%. Moreover, the present method showed to be robust for the three factors considered: the batch of the graphitized carbon cartridges, the flow rate of the sample through the cartridge, and the final redissolved water volume after SPE treatment, which permits its validation. The validated method has been applied to different lyophilized cultures of A. ovalisporum (LEGE X-001) to evaluate CYN content. This procedure can be used for determining CYN in lyophilized natural blooms samples in environmental studies.

Language: English

Type (Professor's evaluation): Scientific

No. of pages: 8