Solid-phase extraction-fluorimetric high performance liquid chromatographic determination of domoic acid in natural seawater mediated by an amorphous titania sorbent

• Published in: Analytica chimica acta 2007-01, Vol.583 (1), p.111-117
• Main Authors: Chan, Ivy O.M., Tsang, Vic W.H., Chu, K.K., Leung, S.K., Lam, Michael H.W., Lau, T.C., Lam, Paul K.S., Wu, Rudolf S.S.
• Format: Article
• Language: English
• Subjects: Algal toxin; Amnesic shellfish poisoning; Analytical chemistry; Applied sciences; Chemistry; Chromatographic methods and physical methods associated with chromatography; Chromatography, High Pressure Liquid - methods; Domoic acid; Exact sciences and technology; Global environmental pollution; Harmful algal blooms; Indicators and Reagents; Kainic Acid - analogs & derivatives; Kainic Acid - analysis; Kainic Acid - isolation & purification; Marine; Marine Toxins - analysis; Marine Toxins - isolation & purification; Other chromatographic methods; Phase Transition; Pollution; Seawater - analysis; Solid-phase extraction; Sol–gel; Spectrometric and optical methods; Spectrometry, Fluorescence; Titania; Titanium
• ISSN: 0003-2670; 1873-4324
• DOI: 10.1016/j.aca.2006.09.063

The feasibility of using sol–gel amorphous titania (TiO 2) as a solid-phase sorbent for the pre-concentration of domoic acid (DA), a potent amnesic shellfish poisoning (ASP) toxin, directly from seawater was explored. The sol–gel titania material is able to adsorb DA from seawater, via the formation of ester-linkage between the carboxylic moieties of DA and the Ti–OH groups on the sorbent surface, at low pH and desorb it at high pH. The chemisorption process is not significantly interfered by the seawater matrix. The optimum pH values for the adsorption and desorption of DA were found to be pH 4 and 11, respectively. The optimal sorbent loading for the batch-type solid-phase extraction of DA was 0.67 mg-TiO 2 ng-DA −1 and adsorption equilibrium was achieved in 2 h at room temperature. The desorbed DA in 500 μL of 0.1 M alkaline borate buffer can be directly derviatized by 4-fluoro-7-nitro-2,1,3-benzoxadiazole (NBD-F) in aqueous media for fluorimetric HPLC quantification. Analyte recovery, repeatability and detection limit of this titania SPE-fluorimetric HPLC determination are 89%, 6.2% and 120 pg-DA mL −1 ( n = 7, P < 0.05), respectively, for a sample volume of 30 mL. This titania SPE technique should also be applicable to the pre-concentration of other polar carboxylate- and phosphonate-containing biomolecules and pharmaceuticals in complex and interfering environmental sample matrices.