title: Improved conditions for the application of solid phase microextraction prior to HPLC-FLD analysis of anatoxin-a.
abstract: Solid phase microextraction coupled with high performance liquid chromatography with fluorescence detection has been optimized and evaluated for a simple, rapid, and selective analysis of anatoxin-a. Four kinds of fiber (100 microm polydimethylsiloxane, 60 microm polydimethylsiloxane/divinylbenzene, 50 microm Carbowax/templated resin-100, and 85 microm polyacrylate) were evaluated for an efficient extraction of the toxin. Parameters relating to the desorption step, such as desorption mode, solvent composition, time for both static and dynamic desorption, as well as carryover, have been studied and optimized. The derivatization process was investigated using NBD-F as derivatizing reagent. Anatoxin-a derivative was formed when the anatoxin-a-loaded fiber was inserted in a vial containing 5 microL of NBD-F. Variables affecting extraction such us ionic strength, temperature, and time have been also optimized. The results obtained showed linearity in the range of 10-2000 ng and a limit of detection of 0.29 ng/mL in river water. The presented method has been applied to different environmental samples.
authors.affiliation: Departamento de Química Analítica y Alimentaria, Facultad de Química, Edificio de Ciencias Experimentales, Universidad de Vigo, Vigo, Spain.
authors.forename: Sandra
authors.initials: S
authors.lastname: Rellán
authors.forename: Ana
authors.initials: A
authors.lastname: Gago-Martínez
mesh_terms: D000180:Acrylic Resins / Q000032:analysis; D002623:Chemistry Techniques, Analytical / Q000379:methods*; D002851:Chromatography, High Pressure Liquid / Q000379:methods*; D003188:Composite Resins / Q000032:analysis; D000458:Cyanobacteria / Q000378:metabolism; D000087522:Cyanobacteria Toxins; D004129:Dimethylpolysiloxanes / Q000032:analysis; D056890:Eukaryota / Q000378:metabolism; D011092:Polyethylene Glycols / Q000032:analysis; D015203:Reproducibility of Results; D012822:Silicon Dioxide / Q000032:analysis; D012828:Silicones / Q000032:analysis; D052617:Solid Phase Microextraction / Q000379:methods*; D012997:Solvents; D020058:Styrene / Q000032:analysis; D013696:Temperature; D013997:Time Factors; D014326:Tropanes / Q000032:analysis*; D015040:Zirconium / Q000032:analysis
chemical_list: D000180:Acrylic Resins; D003188:Composite Resins; D000087522:Cyanobacteria Toxins; D004129:Dimethylpolysiloxanes; D012828:Silicones; D012997:Solvents; D014326:Tropanes; C083568:Z100 composite resin; D011092:Polyethylene Glycols; D020058:Styrene; C006903:carbopol 940; C013830:baysilon; D012822:Silicon Dioxide; C509783:anatoxin a; D015040:Zirconium