A reliable method for the characterisation of vodkas has been developed by application of solid‐phase microextraction (SPME) and gas chromatography/mass spectrometry (GCMS). Sixty‐four samples of commercial Canadian and American vodkas, and one sample each of Japanese and German vodkas, were investigated in this study. The procedure yielded reproducible chromatographic profiles. The detected components were ethyl esters of C8 to C18 fatty acids at μg litre−1 levels, various additives and contaminants. Distinctive profiles were observed for various brands. Markers for differentiating between Canadian and American vodkas were identified. The results of this study indicate that vodkas are differentiated by the combined effects of the original raw materials, any added substances, and differences in processing.
A custom-built ion mobility spectrometer has been used to obtain the IMS spectra of cocaine, heroin, amphetamine sulfate and LSD at different drug concentrations and desorption temperatures. Practical detection limits for these four drugs were obtained as a function of desorber temperature and for heroin as a function of analysis time. Spectral and ionization interferences for each of the four drugs of interest were determined. Spectral interferences by innocuous materials are few; ionization interferences occur only at very high ratios of the mass of innocuous material to that of the drug of interest.
A reliable method based on gas chromatographic/mass spectrometric (GC/MS) profiling of nonvolatile organic acids is described for the characterization of cigars. The method involves an aqueous extraction of ground tobacco and selective isolation of the acids by simply stirring strong anion exchange (SAX) disks in the aqueous tobacco extract. The acids are then directly silylated on the disk with N-methyl-N-trimethylsilyl-trifluroacetamide (MSTFA) in acetonitrile in an autosampler vial. Elution of the derivatized acids in situ allows the sample to be directly analyzed by GC/MS without further sample handling. Compared to the conventional disk-extraction technique using a vacuum manifold, this method is much less labor intensive, and is desirable for multiple sample analysis. Nicotinic acid, succinic acid, glyceric acid, malic acid, pyroglutamic acid, threonic acid, citric acid, uracil, and an unidentified acid were reproducibly quantified in tobacco samples. Principal component analysis (PCA) of the acid profiles of the filler tobaccos of 18 Cuban cigars and 31 non-Cuban cigars shows separation of the two groups, indicating that the acid profiles are potentially useful in the authentication of Cuban cigars.
Ecgonidine methyl ester (EDME), a product of the thermal
decomposition of cocaine, has been identified as a likely
candidate for the detection of concealed cocaine by vapor
sniffing. Using a continuous-flow vapor generator preconcentration/thermal desorption technique in combination with GC-TSD analysis, the vapor pressure of EDME
was measured between −20 and +20 °C, and the results
were fitted into the following equation: log P = 16.6
−
(3.64 × 103/T), where P is in parts
per billion and the
temperature is in kelvin. At 20 °C, the vapor pressure
of
EDME is 16 ppm, approximately 5 orders of magnitude
higher than that of cocaine base.
Direct injection GC/MS was investigated for the analysis of benzyldiethyl(2,6-xylylcarbamoylmethyl)ammonium benzoate (Bitrex), a quaternary ammonium salt, in various Canadian denatured alcohol formulations. Bitrex yielded predominantly a peak due to the neutral diethylamine derivative (I). The structure of I, elucidated by MS and NMR, is strongly related to that of the cation of Bitrex. Compound I was formed from Bitrex in the heated injector port of the GC via a decomposition reaction similar to Stevens rearrangement. The response of I was found to be dependent on the injector port temperature, and the optimal temperature was determined to be in the range 250-350 °C. The GC/MS response of I in SIM mode was used to quantify Bitrex. The effects of the codenaturants sucrose octaacetate (SOA), diethyl phthalate (DEP), and camphor, which are present at much higher concentration than Bitrex in several formulations, were also investigated. The presence of SOA enhanced the response of the analyte considerably, while DEP and camphor had no significant effect. All standard curves of Bitrex (1-16 ppm) in different alcohol matrixes were fitted by second-order polynomial functions, with coefficients of determination (R 2 ) routinely in the range 0.998-0.999. The analysis time was 18 min, and the within-run precision was <4%. The results of this study point to the potential of the GC/MS technique as a quantitative tool for Bitrex in various alcohol formulations.
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