Derivatizing assay for the determination of aldehydes using micellar electrokinetic chromatography

Abstract

In this work, the use of a novel derivatization agent for the determination of aldehydes (in this particular case: formaldehyde, acetaldehyde, propionaldehyde, and valeraldehyde) using micellar electrokinetic chromatography is reported. The derivatization reaction is based on the reaction of aldehydes with benzhydrazide to form the corresponding derivates with maximum absorbance at 250 nm. The experimental conditions of the derivatization reaction as well of the separation were optimized. The adducts were separated with a +22 kV voltage at a temperature of 29°C. The adducts' separation was performed in less than 14 min using as the running buffer a mixture containing 110 mmol/L of sodium dodecyl sulfate and 27 mmol/L of sodium tetraborate at pH 9.45. Samples were injected using hydrodynamic mode (50 mbar × 5 s). The calibration curves were linear up to 15.0 mg/L with r above 0.99. Intra and inter-day precisions were in average 3 and 4%, respectively, and recoveries were in average of 95%. Limits of detection and quantification were around 0.5 and 1.5 mg/L, respectively. The developed method was successfully applied in the analysis of low molar weight aldehydes in yogurt and vinegar samples.

Cyclohexane‐1,3‐dione as a derivatizing agent for the analysis of aldehydes by micelar electrokinetic chromatography with diode array detection

“…However, it was observed insufficient resolution (data not shown) with this electrolyte composition containing only SDS and STB. In MEKC, modifiers, such as β‐cyclodextrin (β‐CD), may serve as a second pseudophase creating an analyte partition between this pseudophase and the micelles which can improve selectivity . Indeed, preliminary experimental work showed satisfactory results using a running electrolyte containing 70 mmol/L of SDS, 29 mmol/L of STB, and 15 mmol/L of β‐CD.…”

Derivatisation for separation and detection in capillary electrophoresis (2015–2017)

“…The handling of minute samples is difficult, and thus this mode is applied when ample volumes of samples and reagents are available. Pre‐capillary mode was the most commonly applied procedure accounting for 2/3 or 29 of the 46 covered articles .…”

“…This is often the case for fluorescence detection where native fluorescence is rather uncommon and only the labelled species provide a strong signal. There were 24 articles on LIF , 16 on UV , 3 on electrochemical detection , and 4 on MS . In MS detection, derivatisation was used to improve the separation (see Section ) and to enable MS detection in favourable positive ion ESI mode .…”

“…Donegatti and co‐workers used the novel benzhydrazide to label four aldehydes in vinegar and yoghurt samples prior to MEKC‐UV at 250 nm . An advantage of using the water‐soluble benzhydrazide was that the aldehyde derivatisation was directly performed of the diluted samples without meticulous sample preparation and completed in 30 min reaction time at room temperature.…”

4-hydrazinobenzoic acid as a derivatizing agent for aldehyde analysis by HPLC-UV and CE-DAD

“…Aldehydes are a group of chemical compounds of the utmost importance in food and environmental science [1,2]. In alcoholic beverages, for example, aldehydes are commonly formed during the fermentation process.…”