The reaction of 1-(2-pyridylazo)-2-acenaphthequinol (PAAL) with cobalt acetate in CHCl 3 gave the complex of Co(PAAL-H) 2 (1), and (PAAL+H) 2 [CoCl 4 ]•2H 2 O (2) was isolated in the same system with ultraviolet light irradiation. Structures of both compounds were determined by X-Ray diffraction. The PAAL ligand was deprotonated in 1, but it further protonated on N position at pyridine group in 2 and form cations. The spectra of these two compounds were also studied, as well as the fluorescence properties. Also, the redox property of 1 was preliminary investigated by cyclic voltammogram.
An improved method was developed for the determination of the four major tobacco-specific nitrosamines(TSNAs) in mainstream cigarette smoke. The new method offers decreased sample preparation and analysis time as compared to traditional methods. This method uses isotope dilution liquid chromatography coupled with a tandem mass spectrometer with electrospray ionization and is significantly more sensitive than traditional methods. It also shows no evidence of artifactual formation of TSNAs. Sample concentrations were determined for four TSNAs in mainstream smoke using two isotopically labeled TSNAs analogues as internal standards. Mainstream smoke was collected on an industry standard 44-mm Cambridge filter pad, extracted with 0.1 mol/L ammonium acetate, purified by solid-phase extraction, and analyzed without further sample cleanup. The analytical column is a 3.9 mm×150 mm Waters Symmertry Shield RP 18 column and volume fraction of the mobile phase is 50% methanol, 50% water containing 0.1% acetic acid. The results show that the linear range is 0.5−100.0 mg/L except for N-nitrosoanabasine (NAB) from 0.25 to 50.0 mg/L. The limits of detection are 0.1 mg/L for N-nitrosonornicotine (NNN), 0.08 mg/L for 4-(methylnitrosamino)-1-(3-py-ridyl)-1-butanone (NNK), 0.05 mg/L for N-nitrosoanatabine (NAT) and 0.06 mg/L for NAB. The recoveries of the four TSNAs are from 90.2% to 105.7%.
This paper reports the analysis of the combustion products from moderate and low-tar cigarettes. The compounds were collected by a solvent trap coupled with automatic headspace solid phase micro-extraction and gas chromatography-mass spectrometry (GC-MS). The fiber, solvent system, extraction temperature, and extraction time were investigated by orthogonal experimental design. The optimized conditions included the use of an 85 lm carboxen/polydimethylsiloxane fiber, tert-butyl methyl ether as the solvent, an extraction temperature of 110 C, and an extraction time of 30 min. Thirty compounds were identified by GC-MS, and twelve aromatic hydrocarbons (51.08%) and 11 hydrocarbons (36.38%) were the major components. The 1,2,3-Trimethylbenzene (79.60%) and furfural (60.03%) had the largest reduction in low-tar cigarettes compared to moderate-tar cigarettes. This method was shown to be fast, simple, accurate, and precise.
A method of gas chromatography-mass spectrometry (GC-MS) with liquid-liquid extraction has been developed for the simultaneous determination of 23 ester compounds including acetate esters, acrylic esters, metacrylic acid esters and phthalate acid esters in cigarette water-borne adhesives. After dispersed in water, the sample was extracted by n-hexane solution containing phenyl ethyl propionate as internal standard substance. Then, the solution was centrifuged and filtrated through a 0.45 microm organic membrane filter. Finally, the solution was separated on a DB-WAXETR column (60 m x 0.25 mm x 0.25 microm), and detected with MS in selected ion monitoring mode, and quantified by internal standard method. The results showed a good linear correlation in the range of 0.4-50.0 mg/L. The recoveries of the ester compounds spiked in the sample were 81.8%-109.1%, and the relative standard deviations (RSDs, n = 5) were less than 4%. The limits of detection (LODs) and limits of quantification (LOQs were in the ranges of 0.02-0.76 mg/kg and 0.04-2.52 mg/kg, respectively. The method is simple, time-saving, and has high sensitivity and good reproducibility. It can be applied to the determination of the 23 ester compounds in cigarette water-borne adhesives.
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