天然和人工培植红景天挥发油的对比研究

应用ＧＣ－ＭＳ和ＧＣ－ＩＲ两种联机法对比研究了天然和人工培植红景天挥发油、分别鉴定出２７个和２４个化合物。ＭＳ给出结构信息和ＩＲ给出官能团信息相结合，提高了分析测试复杂样品的可靠性。     

气相色谱—微波等离子体发射光谱法研究农药1605与人唾液的相互作用

用ＧＣ－ＡＥＤ联用技术研究了农药１６０５，得到１６０５所含六种元素的元素色谱图，并用该方法研究了人唾液与１６０５的相互作用。     

大气有机物热脱附-全二维气相色谱-火焰离子化分析方法

全二维气相色谱（GC×GC）是20世纪90年代发展起来的具有高分辨率、高灵敏度、高峰容量等优势的分离技术,在我国将其用于大气挥发性有机物（VOCs）研究方面才刚刚起步.本文将GC-GC与氢火焰离子化检测器（FID）联用,构建了用于测量大气有机物的热脱附-全二维气相色谱-氢火焰离子化分析系统（TD-GC×GC-FID）.采用HP-5MS和HP-INNOWAX色谱柱,建立了C5-C15大气有机物分析方法,实现了一次分析过程同时分离非甲烷烃（NMHCs）、含氧挥发性有机物（OVOCs）和卤代烃等多种组分.利用标准物质和四级杆质谱（qMS）进行定性,外标法结合FID质量校正因子定量.目标物在GC-GC谱图中第一和第二维保留时间变化分别小于0.6s和0.02s,峰体积平均相对标准偏差为14.3%,其中烷烃和芳香烃为4.5%.标准曲线r2均值大于0.99,平均检出限为6.04ng,平均回收率为111%.利用该方法检测到2010年1月北京市区大气中400多种有机物（信噪比大于50）,鉴定了其中的103种物质,包括烷烃、烯烃、芳香烃、卤代烃、醛、酮、酯、醇和醚等.所测定有机物平均总浓度为51.3×10-9V/V,其中OVOCs约占51%,芳香烃约占30%,烷烃约占15%,卤代烃和烯烃分别占3%和1%.平均浓度最高的前3个组分是乙醇（9.84×10-9V/V）、丙酮（6.72×10-9V/V）和甲苯（3.48×10-9V/V）.     

Combination of solid-phase extraction-hollow fiber for ultra-preconcentration of some triazole pesticides followed by gas chromatography-flame ionization detection

In this study, an extraction and preconcentration technique using solid-phase extraction (SPE) along with hollow fiber (HF) has been developed as an ultra-preconcentration technique for some triazole pesticides in aqueous samples. Triazole pesticides were employed as model compounds to assess the method and were monitored by gas chromatography-flame ionization detection (GC-FID). Initially, an aqueous solution of target analytes was passed through an RP-8 SPE cartridge and then the adsorbed analytes were eluted with μL amounts of toluene. The collected elute was slowly introduced into an HF that had one end blocked. This allowed precipitation inside the lumen and pores of the HF. Finally, the obtained HF was mounted on a home-made solid-phase microextraction syringe and entered into the GC injection port for thermal desorption-GC analysis. The effect of various experimental parameters including injection port temperature, desorption time, state of HF, washing solvent, elution solvent and its volume, sample volume, etc. were investigated for finding the optimum conditions. The calibration graphs were linear in the ranges of 2-1000 ng/mL (penconazole and hexaconazole), 5-1000 ng/mL (tebuconazole), 15-1000 ng/mL (triticonazole) and the detection limits (LODs) ranged from 0.6 to 4.5 ng/mL. The enhancement factors were in the range of 870-950. The relative standard deviations (RSD%) for five repeated experiments (C=250 ng/mL of each pesticide) varied from 4.5 to 8.7%. The relative recoveries obtained for analytes in grape juice samples, spiked with different levels of each pesticide, were in the range of 87-119%.     

A study of the compositional variation of the essential oil of ylang-ylang (Cananga odorata Hook Fil. et Thomson,formagenuina) during flower development

Volatile secondary metabolites from Colombian ylang-ylang flowers were obtained by combined steam distillation - solvent extraction. The samples were analyzed by high resolution gas chromatography with flame ionization, nitrogen/phosphorus, or mass spectrometric detection. The chemical composition of the oils extracted from flowers at different stages of development differed both qualitatively and quantitatively. The generation of total volatile metabolites, light oxygenated compounds in particular, increased markedly during flower maturation. In this work the quality of the ylang-ylang essential oils was studied as a function of flower maturity.     

The analysis of C4–C11 hydrocarbons in naphtha and reformate with a new apolar fused silica column

This paper deals with the separation of alkanes, naphthenes, and aromatic compounds in naphtha and reformate, on a newly developed apolar high resolution GC column. The selectivity of this apolar phase has been compared with those of squalane, DB-1, and SE-30. A total of 95 hydrocarbons were reliably identified, mostly by GC-MS. Repeated measurements of Kováts retention indices are presented as evidence for the reproducible manufacture of fused silica columns coated with this phase.     

Separation and determination of m-phenoxybenzaldehyde reaction products by capillary gas chromatography

A capillary GC method employing an internal standard has been developed and successfully used for quantitative determination both of the raw materials used for the manufacture of m-phenoxybenzaldehyde and for the components of the reaction mixtures obtained at various stages of the development of the process. A complete analysis can be performed in a single temperature programmed run.     

Study on the thermal stability of a chiral stationary phase coated on capillaries for GC

A chiral stationary phase prepared by bonding L -valine-t-butylamide to XE-60 has been coated on glass and metal capillaries. The performances of the chiral glass and metal columns were equivalent to those of commercial fused silica capillary columns. The thermal stability of the glass column was examined up to 280°C. It was found that no appreciable change in separation factor (α value) was observed up to 230°C. The α values gradually decreased between 240 and 260°C, and enantiomer separation was no longer achieved at 280°C. It was concluded that the allowable upper limit temperature of the chiral stationary phase is between 230 and 240°C in the isothermal mode, and ca 260°C in temperature-programmed mode.     

HPLC isolation and NMR structure elucidation of the most prominent octabromo isomer in technical octabromo diphenyl ether

The major octabromo isomer of technical octabromo diphenyl ether mixture (technical octaBDE) DE-79 was isolated by RP-HPLC. Three serially coupled columns (each 250 mm long) enabled a good separation of the target compound from other congeners using 100% ACN as eluent. Approximately 100 microg of the target compound was isolated with a purity of >90% and investigated by MS for confirmation of the degree of bromination. 1H-NMR and 2-D 1H-13C correlation NMR spectra unequivocally clarified that the octaBDE in question is 2,2',3,3',4,4',6,6'-octabromodiphenyl ether (BDE 197). Based on annual production rates of technical BDE products (1999/2001), approximately 380 tons of BDE 197 were annually produced which, on the long term, may enter the environment. Compared with other individual BDE congeners, BDE 197 has the seventh highest application rate. Reductive debromination of BDE 197 can lead to four hepta-, 15 hexa-, 23 penta-, and 28 tetra-BDE isomers, respectively. This variety includes all known major BDEs of environmental concern (BDE 47, 85, 99, 100, 153, 154, and 183). The identification of BDE 197 in technical octaBDE DE-79 strongly suggests that research on the environmental fate of BDEs should include this key-BDE congener.     

云南怒江地区芒果香味的分析

用ＧＣ／ＭＳ方法分析测定了采自云南怒江农场的芒果属（ＭａｎｇｉｆｅｒａＬ）的３个品种三年芒、吕宋芒和马切苏芒的主要香味物质。每个品种的香味成分均在２０个以上。对主要成分进行了半定量计算,结果表明三年芒主要含有异松油烯、γ－羟辛酸内酯、３,７－二甲基－１,３,６－辛三烯、γ－羟己酸内酯、石竹烯、２,６－二叔丁基－４－甲基苯酚;吕宋芒主要含α－蒎烯、蒈烯、２,６－二叔丁基－４－甲基苯酚、石竹烯、γ－羟己酸内酯。