Qingde Su

Comparison of simultaneous distillation extraction and solid-phase microextraction for the determination of volatile flavor components

Traditional simultaneous distillation extraction (SDE) and solid-phase microextraction (SPME) techniques were compared for their effectiveness in the extraction of volatile flavor compounds from various mustard paste samples. Each method was used to evaluate the responses of some analytes from real samples and calibration standards in order to provide sensitivity comparisons between the two techniques. Experimental results showed traditional SDE lacked the sensitivity needed to evaluate certain flavor volatiles, such as 1,2-propanediol. Dramatic improvements in the extraction ability of the SPME fibers over the traditional SDE method were noted. Different SPME fibers were investigated to determine the selectivity of the various fibers to the different flavor compounds present in the mustard paste samples. Parameters that might affect the SPME, such as the duration of absorption and desorption, temperature of extraction, and the polarity and structure of the fiber were investigated. Of the various fibers investigated, the PDMS-DVB fiber proved to be the most desirable for these analytes.

Analysis of free and bound volatiles by gas chromatography and gas chromatography–mass spectrometry in uncased and cased tobaccos

The free and bound volatiles of tobaccos were analyzed by capillary GC and GC-MS. Bound volatiles were isolated by dichloromethane extraction followed by stream distillation continuous extraction (SDE) at pH 2.5 acid hydrolysis. The bound aromatic compounds were hydrolyzed by acid at pH 2.5, and the bound volatiles were liberated and extracted into dichloromethane by SDE simultaneously. In total, 23 volatiles were identified, with neophytadiene, 2-ethyl hexanol, damascenone, benzene ethanol, palmitic acid, stearic acid, linoleic acid, farnesyl acetone, 3-oxo-ionol, and megastigmatrienone being the major components. They consisted mainly of compounds exhibiting aromatic characteristics. The quality and quantity of free and bound volatiles exhibited different distributions in uncased or cased tobaccos. The volatiles existed in higher amounts in bound form than in free form. Compared with uncased tobaccos, free form volatiles showed a decrease after the casing process, while bound volatiles showed an increase.

Determination of pyrethroid residues in tobacco and cigarette smoke by capillary gas chromatography.

The extraction of fenpropathrin, cyhalothrin, cypermethrin, fenvalerate and deltamethrin from tobacco (Nicotina tobaccum) and cigarette smoke condensate with acetone, followed by partition of resulting acetone mixture with petroleum ether, was investigated and found suitable for capillary gas chromatography (GC) residue analysis. Florisil column clean-up was found to provide clean-up procedure for tobacco and cigarette smoke condensate permitting analysis to < or = 0.01 microgram.g-1 for most of the pyrethroids by GC with a 63Ni electron capture detector (GC-ECD). Quantitative determination was obtained by the method of external standards. Cigarettes made from flue-cured tobacco spiked with different amounts of pyrethroids were used and the pyrethroid levels in mainstream smoke were determined. For all the pyrethroid residues, 1.51-15.50% were transferred from tobacco into cigarette smoke.

Determination of acetanilide herbicides in cereal crops using accelerated solvent extraction, solid-phase extraction and gas chromatography-electron capture detector

A method was developed to determine eight acetanilide herbicides from cereal crops based on accelerated solvent extraction (ASE) and solid-phase extraction (SPE) followed by gas chromatography-electron capture detector (GC-ECD) analysis. During the ASE process, the effect of four parameters (temperature, static time, static cycles and solvent) on the extraction efficiency was considered and compared with shake-flask extraction method. After extraction with ASE, four SPE tubes (graphitic carbon black/primary secondary amine (GCB/PSA), GCB, Florisil and alumina-N) were assayed for comparison to obtain the best clean-up efficiency. The results show that GCB/PSA cartridge gave the best recoveries and cleanest chromatograms. The analytical process was validated by the analysis of spiked blank samples. Performance characteristics such as linearity, limit of detection (LOD), limit of quantitation (LOQ), precision and recovery were studied. At 0.05 mg/kg spiked level, recoveries and precision values for rice, wheat and maize were 82.3-115.8 and 1.1-13.6%, respectively. For all the herbicides, LOD and LOQ ranged from 0.8 to 1.7 μg/kg and from 2.4 to 5.3 μg/kg, respectively. The proposed analytical methodology was applied for the analysis of the targets in samples; only three herbicides, propyzamid, metolachlor and diflufenican, were detected in two samples.

Pyrolysis–gas chromatography/mass spectrometry as a useful technique to evaluate the pyrolysis pathways of phenylalanine

Abstract Phenylalanine, a significant amino acid in tobacco, was pyrolyzed in a furnace-type pyrolyzer, using off-line pyrolysis. The pyrolysis temperature was 700xa0°C for simulating the temperature of the pyrolysis zone of cigarette burning. The volatile and semivolatile organic products were trapped by a 0.7xa0m long fused silica capillary with an internal diameter of 0.53xa0mm, and the capillary was immersed in liquid nitrogen during pyrolysis and trap periods. Then, the organic products that were trapped in the capillary were extracted with dichloromethane. The qualitative analysis was carried out by gas chromatography/mass spectrometry (GC/MS). It was found that the experiment apparatus had some advantages, including less secondary reactions and better reproducibility. The typical pyrolysis mechanism of phenylalanine includes: decarboxylation, homolysis, cyclization, deamination, etc.