Determination of anatoxin-a in environmental water samples by solid-phase microextraction and gas chromatography-mass spectrometry.
In the present work, a method was developed and optimized aiming at the determination of anatoxin-a in environmental water samples. The method is based on the direct derivatization of the analyte by adding hexylchloroformate in the alkalinized sample (pH = 9.0). The derivatized anatoxin-a was extracted by a solid-phase microextraction (SPME) procedure, submersing a PDMS fiber in an amber vial for 20 min under magnetic stirring. GC-MS was used to identify and quantify the analyte in the SIM mode. Norcocaine was used as internal standard. The following ions were chosen for SIM analyses (quantification ions in italics): anatoxin-a: 191, 164, 293 and norcocaine: 195, 136, 168. The calibration curve showed linearity in the range of 2.5-200 ng/mL and the LOD was 2 ng/mL. This method of SPME and GC-MS analysis can be readily utilized to monitor anatoxin-a for water quality control.
Rodríguez
Vania
V
Departamento de Análises Clinicas e Toxicológicas, Faculdade de Ciências Farmacêuticas, Universidade de São Paulo, São Paulo, Brasil.
Yonamine
Mauricio
M
Pinto
Ernani
E
D001427:Bacterial Toxins / Q000032:analysis* / Q000592:standards; D019086:Bridged Bicyclo Compounds, Heterocyclic; D000087522:Cyanobacteria Toxins; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods* / Q000592:standards / Q000706:statistics & numerical data; D007202:Indicators and Reagents; D008387:Marine Toxins / Q000032:analysis* / Q000592:standards; D012015:Reference Standards; D052617:Solid Phase Microextraction / Q000379:methods*; D014326:Tropanes / Q000032:analysis* / Q000592:standards; D014874:Water Pollutants, Chemical / Q000032:analysis*
D001427:Bacterial Toxins; D019086:Bridged Bicyclo Compounds, Heterocyclic; D000087522:Cyanobacteria Toxins; D007202:Indicators and Reagents; D008387:Marine Toxins; D014326:Tropanes; D014874:Water Pollutants, Chemical; C509785:anatoxin-a(s); C524097:homoanatoxin-a; C509783:anatoxin a