烟用香料配制的气相色谱法质量控制研究

采用气相色谱法对香料房卷烟用料液中的溶剂及水分进行检测,分析测定其中的水分、乙醇、丙二醇、山梨醇等的含量,通过对香料房每批配制料液的抽检,可以跟踪料液配制的准确性,保证卷烟产品质量,该方法操作简单、准确性高、重现性好。     

GC/MS characterization of mate tea leaves extracts obtained from high-pressure CO2 extraction

This work presents a study concerning the chemical characteristics and analytical separation process of the essential oil obtained from high-pressure carbon dioxide extraction of Ilex paraguariensis. The experiments were performed in a laboratory-scale unit in the temperature range of 20–40 °C, from 100 to 250 bar. A blend of the I. paraguariensis extracts was percolated through a preparative chromatographic column, containing silica gel, and successively eluted with 150 mL of each of the following solvents: hexane, toluene, dichloromethane, ethyl acetate, acetone and methanol. The raw extract and its fractions were analyzed by gas chromatography coupled to mass spectrometry detection (GC/MS). The fractionation procedure showed to be a good clean up technique due to the isolation of different classes of compounds in each fraction. Chromatographic analyses allowed the identification of caffeine, fatty acids and esters, phytol, squalene, Vitamin E, stigmasterol derivatives and saturated hydrocarbons.     

气相色谱在线分析变压吸附法制纯氢中的总碳

利用带镍加氢转化炉的气相色谱仪 ,在线分析变压吸附法制纯氢中的总碳。该法用变压吸附法制的纯氢作燃气 ,在检测器前端将氢气中的CO和CO2 转化为CH4,然后用氢火焰离子化检测器检测 ,直接以检测器的信号 (mV)进行定量。当氢气中总碳体积分数在 1 9～ 5 0 0 μl/L时 ,FID信号值与总碳体积分数有良好的线性关系。方法回收率为 99 90 %～ 10 1 9%,相对标准偏差 <1%。     

Thermal degradation of cinnamoylated poly(vinyl alcohol)

Thermogravimetry and pyrolysis in combination with gas chromatography and infrared spectroscopy were the experimental techniques applied to the thermal degradation of cinnamoylated poly(vinyl alcohol) samples, constituted from vinyl alcohol-vinyl cinnamate photocrosslinkable copolymers. The thermal decomposition products include gases, liquids and solids. The gases are formed from saturated and unsaturated volatile hydrocarbons C₁? C₄, carbon monoxide and carbon dioxide. The liquid fraction includes aromatic hydrocarbons and some oxygenated organic compounds. The solid product identified in the greatest amount was cinnamic acid. The content in the thermal decomposition products varies considerably both with copolymer composition and temperature.     

合成叔十二碳硫醇的填充柱气相色谱分析

讨论了以硫化氢和十二碳烯为原料 ,以固体酸为催化剂 ,采用滴流床反应器连续法合成叔十二碳硫醇工艺中叔十二碳硫醇合成液 (粗硫醇 )的快速分析方法。对采用毛细管柱气相色谱和填充柱气相色谱分析粗硫醇的方法进行了比较。结果表明 ,采用填充柱气相色谱法分析粗硫醇 ,方法简便、快速、可靠 ;完成一次分析只需 1min ,相对标准偏差小于 1%。     

Preparation of fatty acid methyl esters for gas-chromatographic analysis of lipids in biological materials

Theoretically, preparation of fatty acid methyl esters (FAMEs) deals with reversible chemical reactions in a complex system. Methodologically, there are numerous ways, generally characterized by the type of catalysts used and steps involved. Although there are more than a half dozen common catalysts, the majority fall into either acidic (HCl, H₂SO₄ and BF₃) or alkaline types (NaOCH₃, KOH and NaOH), with each having its own catalytic capability and application limitations. In terms of steps, many conventional methods, including those officially recognized, consist of drying, digestion, extraction, purification, alkaline hydrolysis, transmethylation/methylation and postreaction work-up. Although these methods are capable of providing reliable estimates if some precautions are taken, they are cumbersome, time-consuming and cost-inefficient. A new approach has been to transmethylate lipidsin situ. Due to its simplicity, high sensitivity, comparable reliability and capability to determine total fatty acids, the method of direct transmethylation is finding a unique place in lipid determination. Regardless of which method is used, quantitative methylation requires chemists to take precautions at every step involved, particularly during FAME formation and subsequent recovery steps. Evidently, there is an urgent need for more systematic studies, guided by the chemical principle of reactions involved and physicochemical properties of regents and end products, into factors affecting these steps. Hopefully, this will lead to an improved method, which measures lipid composition in biological materials not only with high accuracy but also with high efficiency and minimum costs.     

叔丁醇氧化产物的气相色谱分析

介绍了用气相色谱分析叔丁醇两步氧化制甲基丙烯酸液相产物的组成，该分析方法能够分析液相产物中的醛类，酮类和酸类化合物共计9个组分，C2－C4有机酸无记忆效应，其色谱峰不拖尾，该分析方法的相对标准偏差≤8．5％，回收率在94．5％－103．7％之间，是一种快速，准确，操作简单的分析方法。     

Rapid analysis of polymer homologues and additives with SFE/SFC-MS coupling

A rapid and easy analysis method for polymers is presented. The method involves sample preparation by SFE, separation of the extracted compounds by SFC and simultaneous quantitative detection by FID, as well as identification of unknowns by MS. The applications illustrate how structural research work and routine polymer analysis can be done with this time saving method.     

Volatile constituents of palm wine and palm sap

Palm wine and pasteurised palm sap volatiles were collected, concentrated on a Tenax GC and analysed by gas chromatography and gas chromatography-mass spectrometry. Eighty-two components were identified: 47 esters, 9 alcohols, 5 acids, 6 carbonyls, 2 acetals, 4 terpenes and 9 hydrocarbons. These had all been found previously in conventional wines. Odour evaluation of the separated palm wine components as they eluted suggested that no one compound is responsible for the characteristic palm wine odour. The acetates of higher alcohols and the ethyl esters of straight-chain aliphatic C₆-C₁₀ acids seemed to be important and may play a big role in imparting the fruity nuances of characteristic palm wine odour. Their association with alcohols seemed also to be necessary for the expression of typical palm wine odour. The qualitative difference between palm sap aroma and palm wine aroma appeared to be due mainly to the presence of these esters and alcohols in palm wine and their apparent absence from palm sap, as well as to the presence of some low-boiling esters and alcohols in palm sap and their apparent absence from palm wine.