Gas chromatographic-mass spectrometric analysis of volatile constituents in saliva

Present methods for the development of metabolic profiles are limited to the use of headspace techniques and solvent extraction methods. A new method for the development of saliva profiles which provides information complementary to existing analyses has been developed. The results of the developed methodology provide a reliable, reproducible method for metabolic profiling. Gas chromatographic-mass spectrometric analysis of the volatile constituents provided positive identification of 39 compounds. Application of the developed protocol toward the investigation of saliva as a vehicle for the non-invasive detection of certain pathological states, specifically diabetes mellitus and liver disorders, may be possible.     

Gas chromatographic determination of volatile anaesthetic agents in blood. Part 2. Clinical studies

A method is described for the direct determination of the volatile anaesthetics halothane and isoflurane in blood by gas chromatography with flame-ionisation detection. The method is accurate and precise and allows rapid measurements of blood levels of anaesthetic agents. Headspace concentrations of anaesthetic agents in the concentration range 0-3% V/V are determined with an accuracy of +/- 0.01% V/V. The relative standard deviation of these results is less than 4.0%. A relatively small volume of blood is required for each determination, a factor of great significance in the treatment of children. The need for separate blood calibration graphs for each patient is discussed, further emphasising the need for a rapid calibration procedure. The results from the clinical application of this method show conclusively its suitability for the management of anaesthetised subjects.     

Gas chromatographic determination of volatile alkenes with on-column bromination and electron-capture detection

A method is described for the gas chromatographic-electron-capture detection determination of alkenes via on-column bromination reactions. Pyridinium bromide perbromide (PBPB) was used as the Br₂ source, and a cholesterol-glass beads mixture, treated with methanol, was used to remove excess Br₂. The optimum ratio of cholesterol to glass beads was found to be 1:10, at which 93% of the bromine released from PBPB can be removed, without removal of the derivitized analytes. The conversion efficiency of alkene to the brominated derivative is extremely low (less than 2%) for ethene, whereas for propene and 1-butene it is 41 and 79%, respectively. For C₃---C₅ alkenes, this method is 200–300 times more sensitive than analysis of the underivitized analytes by using conventional flame ionization detection.     

Gas chromatographic determination of volatile alkenes by on-column bromination and electron-capture detection

A method is described for the GC-electron-capture detection determination of ultra trace quantities of alkenes via on-column bromination reactions. Copper bromide coated onto a non-polar solid support, Gas Chrom Q (100–120 mesh) acted as the bromine source. At a temperature of 90–110°C, steel wool may be used to remove selectively up to 90% of the bromine bleed from the reactor. The conversion efficiency of an alkene to the dibrominated derivative is extremely high, up to 90% for ethene, propene, butene and pentene. The bromination of acetylene is also possible, but is not as efficient.     

Gas chromatographic study of the volatile products from co-pyrolysis of coal and polyethylene wastes

The aim of this study was to determine the volatile products distribution of co-processing of coal with two plastic wastes, low-density polyethylene from agriculture greenhouses and high-density polyethylene from domestic uses, in order to explain the observed decrease in coal fluidity caused by polyethylene waste addition. Polymeric materials, although they are not volatile themselves, may be analysed by gas chromatography through the use of pyrolysis experiments. In this way, a series of pyrolysis tests were performed at 400 and 500 degrees C in a Gray-King oven with each of the two plastic wastes, one high-volatile bituminous coal and blends made up of coal and plastic waste (9:1, w/w, ratio). The pyrolysis temperatures, 400 and 500 degrees C, were selected on the basis of the beginning and the end of the coal plastic stage. The organic products evolved from the oven were collected, dissolved in pyridine and analysed by capillary gas chromatography using a flame ionization detector. The analysis of the primary tars indicated that the amount of n-alkanes is always higher than that of n-alkenes and the formation of the alkenes is favoured by increasing the pyrolysis temperature. However, this effect may be influenced by the size of the hydrocarbon. Thus, the fraction C17-C31 showed a higher increase of n-alkenes/n-alkanes ratio than other fractions. On the other hand, the difference between the experimental and estimated values from tars produced from single components was positive for n-alkanes and n-alkenes, indicating that co-pyrolysis of the two materials enhanced the chemical reactivity during pyrolysis and produced a higher conversion than that from individual components.     

Gas chromatographic-mass spectroscopic identification of volatile oil constituents of Omphalocarpus procesum

Summary The steam volatile oil of the seeds ofOmphalocarpus procerum P. Beauv (Sapotaceae) was investigated by capillary gas chromatography with characterisation by mass spectroscopy. The identification of palmitic acid (8%), indole (2.6%), δ-cadinene (7%), cinnamic alcohol (2.12%), α-humulene (0.38%), γ-muurolene (0.49%) as well as smaller amounts of 25 additional compounds was confirmed by GC-MS. In all about 70 compounds were detected in the volatile oil which also contained a large fraction of oxygenated sesquiterpenes.     

Gas chromatographic determination of volatile anaesthetic agents in blood. Part 1. Preparation of standard gas mixtures of volatile anaesthetic agents

A method for preparing standard gas mixtures of the volatile anaesthetics halothane, enflurane and isoflurane is described. Static mixtures of gases of known concentration can be prepared manometrically by measuring the required pressure of anaesthetic gas into a bulb and diluting to atmospheric pressure with air. Standard gas mixtures in the concentration range 0-4% V/V can be prepared with an accuracy of +/- 0.01% V/V, and the relative standard error of measurements of a single standard concentration is less than 0.8%. Significant adsorptive losses in the gas sampling valve were observed for gas standards prepared in the absence of any diluent gas. These losses were not detected for measurements of standards made up to atmospheric pressure in air. A comparison with calibration procedures currently in practice is presented.     

Gas chromatographic study of volatile oxides and hydroxides of Re, Tc, Os, Ru and Rr-II Thermochromatographic investigations

The enthalpies and entropies of absorption on quartz granules of the oxides and hydroxides of Re, Tc, Os, Ru and Ir have been determined by thermochromatography. The separations of these elements have been achieved with dry and moist oxygen as reactive and carrier gas.     

Gas chromatographic determination of volatile congeners in spirit drinks: interlaboratory study

An interlaboratory study of a gas chromatographic (GC) method for the determination of volatile congeners in spirit drinks was conducted; 31 laboratories from 8 countries took part in the study. The method uses GC with flame ionization detection and incorporates several quality control measures which permit the choice of chromatographic system and conditions to be selected by the user. Spirit drink samples were prepared and sent to participants as 10 blind duplicate or split-level test materials for the determination of 1,1-diethoxyethane (acetal), 2-methylbutan-1-ol (active amyl alcohol), 3-methylbutan-1-ol (isoamyl alcohol), methanol (methyl alcohol), ethyl ethanoate (ethyl acetate), butan-1-ol (n-butanol), butan-2-ol (sec-butanol), 2-methylpropan-1-ol (isobutyl alcohol), propan-1-ol (n-propanol), and ethanal (acetaldehyde). The precision of the method for 9 of the 10 analytes was well within the range predicted by the Horwitz equation. The precision of the most volatile analyte, ethanal, was just above statistically predicted levels. This method is recommended for official regulatory purposes.     

基于挥发性组分的气相色谱指纹图谱评价沉香化气片质量

建立了沉香化气片的气相色谱指纹图谱,并结合化学模式识别评价20批沉香化气片的质量。乙醇超声提取20批沉香化气片的挥发性成分,以正十八烷为内标,分析了3个主要组分的含量,且以内标计算其他各组分的相对峰面积,建立了沉香化气片的气相色谱指纹图谱,确定了11个共有峰,得到了各批次样品的相似度,并通过气相色谱-质谱法和对照品比对对10个共有峰进行了指认。将获得的峰面积指纹图谱采用系统聚类分析和主成分分析进行化学模式识别研究,实现了不同批次沉香化气片的区分,发现了造成不同批次样品差异的主要标记物。该方法有效且综合性强,为科学评价与有效控制沉香化气片的质量提供了可靠的参考。     

Rapid automated high-performance liquid chromatographic analysis of cyclic adenosine 3',5'-monophosphate. Synthesis in brain tissues

A rapid and sensitive automated system for measuring cyclic adenosine 3',5'-monophosphate (cAMP) synthesized from either radiolabelled adenine or adenosine 5'-triphosphate (ATP) in intact and broken cell tissue preparations, respectively, is described. After incubation with radiolabelled precursor, tissue samples are deproteinized and then injected directly onto a reversed-phase high-performance liquid chromatographic column. The column effluent fraction which contains cAMP is collected into scintillation vials and assayed for tritium by liquid scintillation spectrometry. Since the high-performance liquid chromatographic and fraction collection procedures are automated, over fifty samples can be analyzed in duplicate in a single day. The utility of this assay is illustrated by investigations of the effects of beta-adrenergic receptor stimulation on cAMP synthesis in tissue slices prepared from rat cerebral cortex and dopamine on cAMP synthesis in striatal membrane preparations.     

Gas chromatographic study of volatile oxides and hydroxides of Tc, Re, Ru, Os and Ir-I Investigation by isothermal gas chromatography

Traces of radioactive elements were produced by the irradiation of uranium foils (93% (235)U) with thermal neutrons, and of gold foils with 600-MeV protons. They were volatilized as oxides and hydroxides by heating at 1500 degrees in an O(2) or O(2)/H(2)O stream and separated by adsorption chromatography on quartz granules. Compounds in the effluent gas were detected with a Ge(Li) detector and the elements identified by gamma-spectrometry.     

Major volatile constituents of Annona squamosa L. bark

The volatile constituents of Annona squamosa L. bark were identified from the essential oil obtained by steam distillation and studied by GC/MS. Six major components were identified as 1H-Cycloprop(e)azulene (3.46%), germacrene D (11.44%), bisabolene (4.48%), caryophyllene oxide (29.38%), bisabolene epoxide (3.64%) and kaur-16-ene (19.13%). The oil was also screened for its antimicrobial activity, which exhibited a significant antimicrobial activity against Bacillus subtilis and Staphylococcus aureus.