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Headspace solid‐phase microextraction with on‐fiber derivatization for the determination of aldehydes in algae by gas chromatography–mass spectrometry
Author(s) -
Ma Jiping,
Xiao Ronghui,
Li Jinhua,
Li Jie,
Shi Benzhang,
Liang Yanjuan,
Lu Wenhui,
Chen Lingxin
Publication year - 2011
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.201000860
Subject(s) - derivatization , chromatography , solid phase microextraction , chemistry , gas chromatography–mass spectrometry , extraction (chemistry) , mass spectrometry , gas chromatography , detection limit , fiber , divinylbenzene , organic chemistry , styrene , copolymer , polymer
A simple, fast, sensitive and cost‐effective method based on headspace solid‐phase microextraction (HS‐SPME) with on‐fiber derivatization coupled with gas chromatography–mass spectrometry was developed for the determination of six typical aldehydes, 2 E ‐hexenal, heptanal, 2 E ‐heptenal, 2 E ,4 E ‐heptadienal, 2 E ‐decenal and 2 E ,4 E ‐decadienal in laboratory algae cultures. As derivatization reagent, O ‐2,3,4,5,6‐(pentafluorobenzyl) hydroxylamine hydrochloride, was loaded onto the poly(dimethylsiloxane)/divinylbenzene fiber for aldehydes on‐fiber derivatization prior to HS‐SPME. Various influence factors of extraction efficiency were systematically investigated. Under optimized extraction conditions, excellent method performances for all the six aldehydes were attained, such as satisfactory extraction recoveries ranging from 67.1 to 117%, with the precision (relative standard deviation) within 5.3–11.1%, and low detection limits in the range of 0.026–0.044 μg/L. The validated method was successfully applied for the analysis of the aldehydes in two diatoms ( Skeletonema costatum and Chaetoceros muelleri ), two pyrrophytas ( Prorocentrum micans and Scrippsiella trochoidea ) and Calanus sinicus eggs (feeding on the two diatoms above).