Solid-phase Microextraction of Volatile Polar Compounds in Water

Analysis of phenolic acids as chloroformate derivatives using solid phase microextraction–gas chromatography

A headspace solid-phase microextraction (SPME) method was developed for the determination of secondary compounds from Brazilian sugar cane spirits, or cachaça, by GC-FID. An SPME holder with an 85 microm polyacrylate coating was utilized. The novel method is compared with an optimized method: liquid-liquid extraction (LLE). Both methods showed good linearity, but the repeatability for analyses done with the SPME technique (%RSD = 1.8-3.9) was better than for those done with LLE (%RSD = 10.3-11.7). The concentrations of the analytes obtained in the analysis of 12 cachaça samples with the SPME technique were higher than those obtained with LLE. In the SPME method the extraction wastes are smaller. Cachaça samples were qualitatively analyzed for GC-MS.

Chloroform and methylene chloride were extracted from human whole blood and urine by headspace solid phase microextraction (SPME) using a Carboxen/polydimethylsiloxane (Carboxen/PDMS) fibre before capillary gas chromatography (GC)/flame ionization detection (FID). Whole blood or urine was placed in a vial and mixed with distilled water. The vial was heated at 30 degrees C, and the solvents were extracted from the headspace by SPME. The extraction efficiencies of chloroform and methylene chloride from whole blood were 40.3% and 35.8%, respectively; those for urine were 57.0% and 43.6%, respectively. The calibration curves for chloroform were linear in the range of 1-8 micrograms/ml for blood and urine samples, and those for methylene chloride in the range of 0.5-8 micrograms/ml. The detection limits for both compounds were 0.3 microgram/ml for whole blood and 0.2 microgram/ml for urine. The headspace SPME with Carboxen/PDMS fibre coupled with GC/FID seems useful for analyses of chloroform and methylene chloride in forensic toxicology and environmental chemistry.

Sample preparation is important for the isolation and concentration of desired trace components from complex matrices. Sample preparation is the most labor-intensive and error-prone process in analytical methodology, and greatly influences the reliable and accurate determination of analytes. The integration of sample preparation with various analytical instruments is most conveniently achieved by using microextraction techniques and/or microdevices. Solid-phase microextraction (SPME) is both simple and effective, enabling miniaturization, automation and high-throughput performance. Moreover, SPME has reduced analysis times, as well as the costs of solvents and disposal. This review describes current developments and future trends in novel SPME techniques, including fiber SPME, in-tube SPME and related new microextraction techniques. Especially innovative SPME approaches, including multi-well high-throughput sampling, ligand-receptor binding study for pharmacokinetics, direct in vivo sampling, chip-based microfluidic system, and new sampling techniques using intelligent carbon nanotube and temperature-response polymer in pharmaceutical and biomedical analysis are focused items.

Analysis of methanol or formic acid in body fluids by headspace solid-phase microextraction and capillary gas chromatography

The profile of volatile compounds of yellow passion fruit juice was analyzed by solid phase microextraction headspace (HS-SPME) and optimized static headspace (S-HS) extraction techniques. Time, temperature, NaCl concentration and sample volume headspace equilibrium parameters was adjusted to the S-HS technique. The gaseous phase in the headspace of samples was collected and injected into a gas chromatograph coupled to a mass spectrometer. In the HS-SPME technique was identified 44 volatile compounds from the yellow passion fruit juice, but with S-HS only 30 compounds were identified. Volatile esters were majority in both techniques, being identified ethyl butanoate, ethyl hexanoate, (3z)-3-hexenyl acetate, hexyl acetate, hexyl butanoate and hexyl hexanoate. Aldehydes and ketones were not identified in S-HS, but were in HS-SPME. β-Pinene, p-cymene, limonene, (Z)-β-ocimene, (E)-β-ocimene, γ-terpinene, α-terpinolene and (E) -4,8-dimethyl-1, 3,7 - nonatriene terpenes were identified in both techniques. This study showed that the S-HS optimized extraction technique was effective to recovery high concentrations of the major volatile characteristics compounds in the passion fruit, such as ethyl butanoate and ethyl hexanoate, which can be advantageous due to the simplicity of the method.

Analysis of volatile compounds of pineapple wine using solid-phase microextraction techniques

In-Groove Carbon Nanotubes Device for SPME of Aromatic Hydrocarbons

Development of a solid phase microextraction gas chromatography tandem mass spectrometry method for the analysis of UV filters

Headspace solid-phase microextraction and gas chromatographic determination of dinitroaniline herbicides in human blood, urine and environmental water

An approach to solventless sample preparation procedure for pesticides analysis using solid phase microextraction/supercritical fluid extraction technique

Porous material-based sorbent coatings in solid-phase microextraction technique: Recent trends and future perspectives

A fast testing procedure for the determination of VOCs in textile matrix using solid phase microextraction (SPME) and gas chromatography-mass spectrometry (GC-MS) was introduced. Samples were cut into small pieces and soaked in 5% methanol (v/v) saturated NaCl solution with supersonic pretreatment at 40±1°Cwater-bathing for 15 min and headspace exposure for 10 min at 50°C with stirring rate at 1100rmp. The influence of SPME adsorption time, stir speed, adsorption time and temperature, and gas chromatography (GC) inlet conditions for the SPME were investigated. Then the matrix solutions were extracted by headspace SPME and analysis by GC/MS. Under the optimized conditions, the limits of detection for target compounds were 0.005mg/kg with average recovery between 90.6-108.7%. The results obtained clearly showed the potential of SPME for efficient concentration of the target compounds and also demonstrated the reliability of this extraction technique for the monitoring of textile quality for the eco-marks.

2 - Theory of Solid-Phase Microextraction

Preliminary study of solid phase micro-extraction (SPME) as a method for detecting insect infestation in wheat grain