树脂酸性组分的氢氧化四甲铵甲基化与GC-MS分析

利用氢氧化四甲铵(TMAH)对马尾松树脂(塔罗油)进行甲基化，并对其产物进行GC—MS分析；研究表明TMAH甲基化后进行GC—MS分析是测定树脂中酸性组分的一种快速有效的方法，但酸性组分中的脂肪酸要比树脂酸难于甲基化，因此为了确保甲基化反应完全，应适当延长甲基化反应时间。     

毛细管色谱法分析糠醛中组分

选择最佳GC／MS分析条件，对工业级和分析级糠醛所含各组分进行分离和检测，通过质谱谱库的计算机检索，结合图谱解析和参考文献定性，鉴定出了十个主要组分。在气相色谱仪上，采用内标法对各组分进行定量，取得了满意的分析结果。     

猪油样品中有机锡化合物的气相色谱-火焰光度法及气相色谱-质谱联用分析

通过将污染猪油中的有机锡化合物进行丙基化衍生后,利用气相色谱－ 火焰光度法（GC－FPD）及毛细管气相色谱－质谱联用（GC－MS）对它们作了全面的定性分析。实验结果表明：猪油样品中均含有二甲基锡,多数样品中还含有三甲基锡和一甲基锡。     

93号汽油样品组分的GC-MS分析

采用气相色谱-质谱法(GC—MS)在DB-5石英毛细管柱上对93号汽油样品进行了分析，检出94种组分；用归一化法进行定量，分析了其中的烯烃化合物，对于汽油生产中控制和降低汽油中烯烃含量有较好的实际意义。     

全二维气相色谱/飞行时间质谱用于莪术挥发油分离分析特性的研究

用全二维气相色谱 /飞行时间质谱 (GC×GC/TOFMS)研究莪术挥发油。对GC×GC与GC的分离特性和GC×GC/TOFMS与GC/MS的定性能力进行了比较。在相同条件下 ,GC分离出 87个峰 ,GC×GC分出约 5 0 0个峰 ,GC/MS和GC×GC/TOFMS鉴定出匹配度大于 80 0的组分分别为 4 6种和 2 2 7种。除此之外 ,GC×GC/TOFMS对每一个组分可给出三维定性信息 ,定性可靠性大大提高。研究结果显示与传统的分析技术相比 ,GC×GC/TOFMS在中药挥发油成分分析领域有很大的优势     

水体中有机污染物的分析

采用大孔径树脂吸附法对地表水和地下水中微量有机污染物进行富集，再用GC—MS法进行分析，其中地表水样品中共检出有机污染物42种，两处地下水样品中分别检出有机污染物9种和10种。对地表水与地下水之间相关性的研究表明，地下水样品中捡出的有机污染物都包括在地表水所含有机污染物的范围之内，地下水中含有有机污染物与地表水受到污染存在支接联系。     

多种气相色谱联用技术分析陕西刺五加茎挥发油的化学成分

采用气相色谱/四极杆质谱(GC/qMS)、气相色谱/正交加速飞行时间质谱(GC/oaTOFMS)和气相色谱/傅里叶变换红外光谱(GC/FTIR)联用技术,对一种陕西产刺五加Acanthopanax senticosus (Rupr. et Maxim.) Harms茎挥发油的化学成分进行了分析。基于GC/qMS谱库的检索功能,结合GC/FTIR在结构鉴别上的优势和GC/oaTOFMS对质谱碎片离子精确的质量测定功能,成功地实现了对68个色谱组分的定性分析。与使用单一的联用技术(例如GC/qMS)相比,利用多种色谱联用技术在定性分析上的互补性,可以明显提高对组成复杂的挥发油类样品分析的可靠性。     

同时裂解甲基化气相色谱法鉴别合成胶粘剂

 应用同时裂解甲基化气相色谱法 (Py Me GC)对合成胶粘剂进行了鉴别。采用热丝型裂解器、氢火焰离子化气相色谱仪、FFAP毛细管柱、程序升温方式及季铵盐甲基化试剂 ,对刑事案件中常见的丙烯酸酯类及其改性体、醋酸乙烯酯、聚乙烯醇等合成胶粘剂进行了测定 ,并对样品裂解各主要组分峰进行了GC/MS定性分析 ,同时比较了相同样本用常规裂解气相色谱法 (Py GC)测定的结果。结果表明 :Py Me GC法比Py GC法可获得更多的物质组分信息 ,是一种适用于法庭科学鉴定的方法。     

广东土牛膝超临界流体萃取物的 GC-MS分析

采用GC－MS技术,对广东土牛膝的超临界流体萃取物中的化学成分进行了分析。气相色谱分离出77种组分,鉴定出其中32种化合物,主要为萜类物质（大部分为倍半萜）、有机酸及其酯类、酚类等化合物。     

兴奋剂中利尿剂的检测方法

利尿剂是国际奥委会医学委员会禁止使用的一类兴奋剂。该文对兴奋剂中利尿剂的检测方法进行了综述,重点阐述了样品的处理方法,HPLC－GC－MS的检测方法及各种衍生化方法。     

Comparison of different mass spectrometry techniques in the measurement of L‐[ring‐13C6]phenylalanine incorporation into mixed muscle proteins

Precise measurement of low enrichment of stable isotope labeled amino‐acid tracers in tissue samples is a prerequisite in measuring tissue protein synthesis rates. The challenge of this analysis is augmented when small sample size is a critical factor. Muscle samples from human participants following an 8 h intravenous infusion of L‐[ring‐¹³C₆]phenylalanine and a bolus dose of L‐[ring‐¹³C₆]phenylalanine in a mouse were utilized. Liquid chromatography tandem mass spectrometry (LC/MS/MS), gas chromatography (GC) MS/MS and GC/MS were compared to the GC‐combustion‐isotope ratio MS (GC/C/IRMS), to measure mixed muscle protein enrichment of [ring‐¹³C₆]phenylalanine enrichment. The sample isotope enrichment ranged from 0.0091 to 0.1312 molar percent excess. As compared with GC/C/IRMS, LC/MS/MS, GC/MS/MS and GC/MS showed coefficients of determination of R² = 0.9962 and R² = 0.9942, and 0.9217 respectively. However, the precision of measurements (coefficients of variation) for intra‐assay are 13.0%, 1.7%, 6.3% and 13.5% and for inter‐assay are 9.2%, 3.2%, 10.2% and 25% for GC/C/IRMS, LC/MS/MS, GC/MS/MS and GC/MS, respectively. The muscle sample sizes required to obtain these results were 8 µg, 0.8 µg, 3 µg and 3 µg for GC/C/IRMS, LC/MS/MS, GC/MS/MS and GC/MS, respectively. We conclude that LC/MS/MS is optimally suited for precise measurements of L‐[ring‐¹³C₆]phenylalanine tracer enrichment in low abundance and in small quantity samples. Copyright © 2013 John Wiley & Sons, Ltd.     

用GC-MS、GC-MS-MS方法检测某些有机质成熟度参数的比较

Tm／Ts,C29甾烷ααα20S／(20S+20R)是判断原油成熟度的重要参数。所以能否准确地检测这些化合物就显得尤为关键和重要。以往我们通常采用GC-MS单极质谱来检测原油和烃原岩抽提物中饱和烃里的萜烷和甾烷成分。但利用GC-MS单极质谱分析得到的m／z191质量色谱图中,Tm、Ts往往与三环和四环萜烷同时共流出,以至有时导致假的Tm／Ts比值。利用GC-MS单极质谱分析得到的m／z217质量色谱图中规则甾烷分布受重排甾烷的影响,很难区分C29甾烷和4-甲基甾烷(即没有办法排除共流峰的干扰)。这是因为Tm、Ts和C29甾烷等生物标记化合物在特定的色谱柱中有     

Identification of polymer building blocks by Py–GC/MS and MALDI-TOF MS

The main goal of this work is to identify polyurethane (PU) building blocks by pyrolysis gas chromatography/mass spectrometry (Py–GC/MS) and matrix-assisted laser desorption/ionization-time of flight mass spectrometry (MALDI-TOF MS). Toluene diisocyanate (TDI) and diphenylmethane diisocyanate (MDI) are widely used polymer building blocks. Py–GC/MS and MALDI-TOF MS were proved to be powerful methods to distinguish TDI-PU and MDI-PU according to the characteristic pyrolysis products and the different repeated units, respectively. In Py–GC/MS, the specific pyrolyzates are TDI for TDI-PU and MDI for MDI-PU. In MALDI-TOF MS, the weights of repeated units are 264?g/mol for TDI-PU and 340?g/mol for MDI-PU.     

Analysis of coal tar and petroleum pitches by computerized pattern recognition

Pyrolysis gas chromatography (P/GC) has been successful in differentiating coal tar pitches which are used in the manufacture of high temperature graphite materials [1,2]. In the present study, coal tar and petroleum pitches received from five suppliers were readily differentiated using three distinct methods of polymer analysis: dynamic headspace and pyrolysis gas chromatography mass spectrometry (DH/GC/MS and P/GC/MS, [3]), and pyrolysis mass spectrometry (P/MS, [4,5]). All of these methods are appropriate for the analysis and pattern recognition study of coal and petroleum products; however, methods which incorporate GC usually necessitate long analysis times and are subject to problems associated with gas chromatographic reproducibility (e.g. active sites [6], and nonconstant retention times). As a fingerprint analysis method, P/MS is rapid and ideally suited to computerized pattern recognition study of pitches due to the simple format of P/MS data (computer tabulation of normalized intensities versus masses); whereas, in the present study, the normalized peak area versus retention time date from DH/GC/MS and P/GC/MS analyses were not suitable for direct input to a computerized pattern recognition analysis program, (due to non-constant retention times and improper data format). One limitation is that P/MS does not provide positive identification of thermally evolved products (as can DH/GC/MS and P/GC/MS) due to the complexity of the spectra of a mixture of compounds produced by P/MS. Within the limits of the commercial instrumentation and computer programs used in this study, a combination of all three techniques provided the greatest capability for the differentiation of the five coal tar and petroleum based pitches studied.     

Metabolite analysis in Curcuma domestica using various GC‐MS and LC‐MS separation and detection techniques

The metabolic profile of polar (methanol) and non‐polar (hexane) extracts of Curcuma domestica, a widely used medicinal plant, was established using various different analytical techniques, including GC‐FID, GC‐MS, HR‐GC‐MS and analytical HPLC‐ESI‐MS/MS by means of LTQ‐Orbitrap technology. The major non‐volatile curcuminoids curcumin, demethoxycurcumin and bisdemethoxycurcumin were identified when their chromatographic and precursor ion masses were compared with those of authentic standard compounds. In this paper we describe for the first time a GC/MS‐based method for metabolic profiling of the hydrophilic extract. We also identified 61 polar metabolites as TMS derivatives. Copyright © 2009 John Wiley & Sons, Ltd.     

Analysis of anabolic steroids in hair by GC/MS/MS

A simple and sensitive gas chromatography/tandem mass spectrometry (GC/MS/MS) method is described for the detection of anabolic steroids, usually found in keratin matrix at very low concentrations. Hair samples from seven athletes who spontaneously reported their abuse of anabolic steroids, and in a single case cocaine, were analyzed for methyltestosterone, nandrolone, boldenone, fluoxymesterolone, cocaine and its metabolite benzoylecgonine. Anabolic steroids were determinate by digestion of hair samples in 1 m NaOH for 15 min at 95 degrees C. After cooling, samples were purificated by solid-phase and liquid-liquid extraction, then anabolic steroids were converted to their trimethylsilyl derivative and finally analyzed by GC/MS/MS. For detection of cocaine and benzoylecgonine, hair samples were extracted with methanol in an ultrasonic bath for 2 h at 56 degrees C then overnight in a thermostatic bath at the same temperature. After the incubation, methanol was evaporated to dryness, and benzoylecgonine was converted to its trimethylsilyl derivative prior of GC/MS/MS analysis. Results obtained are in agreement with the athletes' reports, confirming that hair is a valid biological matrix to establish long-term intake of drugs.     

GC/MS和ESI/MS/MS同位素内标法检测甲基丙二酸血症

以甲基丙二酸血症为对象,分别用GC/MS和ESI/MS/MS方法对该疾病进行了定性和定量检测.通过对样品前处理和分离条件的改善,对疾病的标识化合物之一甲基丙二酸进行了定量测定,其稳定性、精密度和回收率结果很好.同时比较了GC/MS和ESI/MS/MS两种方法的特点,发现两种方法的结合不仅可满足新生儿代谢疾病筛查的要求,同时还可对高危人群进行诊断.     

Optimization of a GC‐MS/MS Method for the Analysis of PCDDs and PCDFs in Human and Fish Tissue

This paper outlines the possibilities of selectivity and sensitivity enhancement in measuring PCDD/F congeners using an ion trap GC‐MS/MS. The pressure of the collision gas and the collision energy were optimized. The modified GC‐MS/MS method was applied to the determination of PCDDs and PCDFs in human and fish tissues. Limits of quantification were about 1 pg/g of fat for all seventeen 2378 PCDD/Fs tested (starting amount of fat, 2 g).     

气相色谱法测邻氰基苄基氯

采用GC／MS法检测出邻氰堪苄基氯中的杂质组分，并使用萘做内标物进行气相色谱法对邻氰堪苄基氯的定量检测。     

毛细管色谱-质谱法测定环境大气中挥发性有机污染物

毛细管色谱-质谱法测定了环境大气中挥发性污染物。用液氧冷冻法和常温吸附法(TenaxGC)分别采集大气样品,然后用两种系统进行浓缩,并进入毛细管色谱-质谱体系,完成了有机污染物的定性定量分析。解决了一些色谱-质谱联用中的问题。并且还讨论了无分流进样问题,比较了两种采样方法。用此方法测定了某炼油厂环境大气中的污染物。