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Determination of anatoxin‐ a in environmental water samples by solid‐phase microextraction and gas chromatography‐mass spectrometry
Author(s) -
Rodríguez Vania,
Yonamine Mauricio,
Pinto Ernani
Publication year - 2006
Publication title -
journal of separation science
Language(s) - English
Resource type - Journals
SCImago Journal Rank - 0.72
H-Index - 102
eISSN - 1615-9314
pISSN - 1615-9306
DOI - 10.1002/jssc.200500488
Subject(s) - solid phase microextraction , chromatography , derivatization , chemistry , analyte , mass spectrometry , gas chromatography–mass spectrometry , gas chromatography , detection limit , calibration curve , selected ion monitoring , sample preparation , analytical chemistry (journal)
Abstract 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.