Headspace single‐drop microextraction with in‐drop derivatization for aldehyde analysis

Abstract

A new technique, headspace single-drop microextraction (HS-SDME) with in-drop derivatization, was developed. Its feasibility was demonstrated by analysis of the model compounds, aldehydes in water. A hanging microliter drop of solvent containing the derivatization agent of O-2,3,4,5,6-(pentaflurobenzyl)hydroxylamine hydrochloride (PFBHA) was shown to be an excellent extraction, concentration, and derivatization medium for headspace analysis of aldehydes by GC-MS. Using the microdrop solvent with PFBHA, acetaldehyde, propanal, butanal, hexanal, and heptanal in water were headspace extracted and simultaneously derivatized. The formed oximes in the microdrop were analyzed by GC-MS. HS-SDME and in-drop derivatization parameters (extraction solvent, extraction temperature, extraction time, stirring rate microdrop volume, and the headspace volume) and the method validations (linearity, precision, detection limit, and recovery) were studied. Compared to liquid-liquid extraction and solid-phase microextraction, HS-SDME with in-drop derivatization is a simple, rapid, convenient, and inexpensive sample technique.

Griess micro-assay for the determination of nitrite by combining fibre optics-based cuvetteless UV–Vis micro-spectrophotometry with liquid-phase microextraction

“…The effect of the sample temperature was studied by exposing the extractant drop in the headspace above an aqueous solution thermostatized at 2-90 • C. An almost linear increase in the analytical signal was observed when the temperature was increased up to 65 • C. However, the extraction efficiency decreases above this temperature, presumably due to the exothermic process involving the dissolution of the analyte in the drop. This is consistent with results obtained in other works [45][46][47]. Consequently, experiments were carried out at 65 • C.…”

Sampling flower scent for chromatographic analysis

“…This higher analyte uptake adds to the sensitivity increases that may result from the chemical nature of the derivative and from the detection system employed. Deng et al [75] used an analogous approach in the hanging-drop liquid-phase microextraction method for aldehydes, in which decane was the solvent and O-2,3,4,5,6-(pentafluorobenzyl)-hydroxylamine hydrochloride was the derivatizing reagent.…”

Rapid analysis of aldehydes by simultaneous microextraction and derivatization followed by GC‐MS

“…The SDME technique has been used for extraction and analysis of different compounds in various samples [18][19][20][21]. Deng et al developed SDME technique for determination of aldehyde in water samples [5]. However, there are some disadvantages in this method; it is difficult to achieve a stable organic drop, formation of air bubbles can occur and extraction is time-consuming and in most cases equilibrium is not attained even after a long time [22,23].…”

“…The determination of low-molecular mass aldehydes present in environmental liquids such as wastewater is becoming an urgent task due to their toxic or carcinogenic characteristics. GC is widely used in the analysis of aldehydes owing to its simplicity, high resolving power, good sensitivity, short analysis time and relatively low cost [2][3][4][5]. However, GC analysis of low-molecular mass aldehydes presents certain difficulties because of their high volatility and polarity.…”