Headspace solid‐phase microextraction with on‐fiber derivatization for the determination of aldehydes in algae by gas chromatography–mass spectrometry

Abstract

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, 2E-hexenal, heptanal, 2E-heptenal, 2E,4E-heptadienal, 2E-decenal and 2E,4E-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 mg/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).

Novel micro‐extraction by packed sorbent procedure for the liquid chromatographic analysis of antiepileptic drugs in human plasma and urine

“…The extraction is based on the partitioning of the analytes between the organic phase on the fused‐silica fibres and the analytes. Many factors, such as pH, temperature, salt concentration and stirring affect the equilibrium constant and the equilibration time 9–15. The major disadvantages of SPME in quantitative analysis are low sensitivity, the frequent inability of the fibre to withstand a complete run and the impossibility of treating samples in an organic solvent.…”

On‐fiber Derivatization for Determination of Ethylene Glycol Concentration in Lubricant oil By SPME‐GC/MS

“…[12][13][14] The mass spectra for EG and CH-one are obtained. The average area response of each fiber for the EG (m/z 31), CH-one (m/z 55), and derivatized EG (m/z 99) base ions is shown in Figure 3.…”

In vivo determination of the volatile metabolites of saprotroph fungi by comprehensive two-dimensional gas chromatography

“…The use of both in vivo and in vitro SPME has been suggested for the isolation of the volatile metabolites from sources ranging from fungi and algae to human subjects, due to its versatility in the extraction of volatile compounds and its ability to limit interferents present in complex matrices by pre‐concentrating analytes that are present even at low concentrations . SPME is an extraction technique that is typically employed when it is necessary to determine the identity of volatile metabolites involved in dynamic processes that occur continuously and systematically, causing no interruption in the living system being investigated .…”