用毛细管GC／MS和GC／FTIR研究挥发油的化学成分

本文用毛细管GC/MS和GC/FTIR对异叶青兰和鼠曲草两种植物挥发油的化学成分进行了研究,讨论了两种方法分析挥发油化学成分的优点和局限性。     

Fused silica capillary column GC/MS for the analysis of priority pollutants

Operational characteristics have been determined for fused silica capillary column (FSCC) GC/MS as applied to “extractable” priority polutants. Chromatographic data show excellent relative retention time (RRT) intralaboratory precision and interlaboratory accuracy when multiple internal standards are empolyed. Potential chromatographic problems, such as column overload and “double peaking”, are addressed. Response factor relative standard deviations (RSD) at 50 ng for most of the extractable priority pollutants over the long term indicated precise determination (i.e. RSD generally ≤ 10%). Linearity was demonstrated over two orders of magnitude for FSCC GC/MS analysis of compounds with relatively low and high RF (response factor) values. Potential quantitative problems, such as saturation, are discussed. For certain aromatic priority pollutants interlaboratory RF agreement was observed. This was noted as perhaps the most important property of FSCC GC/MS analysis when the multiple internal standard approach is utilized. Determinations of extractable priority pollutants are directly compared for paced column GC/MS and FSCC GC/MS analysis of separate and composited extracts. For six extracts analyzed in triplicate, the latter configuration was shown to produce more consistent results. In view of the superior analysis logistics of composite extract FSCC GC/MS analysis, this approach was established as the preferred method for the analysis of priority pollutants classified as extractable.     

调味品中氯丙醇的GC/ECD和GC/MS/MS衍生化检测方法研究及应用

报道了调味品中氯丙醇的衍生化气相色谱(GC／ECD)和衍生化气相色谱双串联质谱法(GC／MS／MS)测定。GC／ECD测定酱油中3—氯—1，2—丙二醇(3—MCPD)的检出限达到0．01mg／kg，回收率为91％～104％，变异系数为2．27％～7．96％；GC／MS／MS同时测定酱油中1，3—二氯—2—丙醇、2，3—二氯—1—丙醇和3—氯—1，2—丙二醇，1，3—二氯—2—丙醇、2，3—二氯—1—丙醇的检出限为0．02mg／kg，3—氯—1，2—丙二醇的检出限为0．01mg／kg，回收率在92％～106％，变异系数为3．51％～13．33％。     

Analysis of turkish lignite tar by coupled LC/GC,GC/MS,and capillary SFC

This work describes the analysis of a pyrolysis product of a lignite sample obtained from the Turkish Goynuk reserve. The aliphatic, aromatic and polar compounds present in the tar are separated and identified by various chromatographic techniques: Capillary gas chromatography/mass spectrometry (GC/MS), on-line high performance microbore liquid chromatography/capillary gas chromatography (LC/GC) and capillary supercritical fluid chromatography (SFC). The suitability of each technique for this particular application is discussed, and semi-quantitative results are presented for the major components detected.     

红景天挥发油的GC／MS／DS和GC／IR／DS研究

红景天挥发油的ＧＣ／ＭＳ／ＤＳ和ＧＣ／ＩＲ／ＤＳ研究阎吉昌，张宏徐少敏卫永弟，阎雪（东北师范大学测试中心，长春，１３００２４）（吉林省石油化工研究院，白求恩医科大学）关键词红景天，色谱／质谱，色谱／红外，复杂有机混合物应用色谱／质谱／计算机（ＧＣ／Ｍ...     

气相色谱-质谱法测定卷烟烟气总粒相物中14种芳香胺

以五氟丙酸酐为衍生化试剂,氘代2-氨基萘和氘代邻甲苯胺为双内标,采用DB-35MS石英毛细管柱(30 m×0.25 mm i.d×0.25 μm d.f)和选择离子模式,建立了卷烟烟气总粒相物中芳香胺的气相色谱-质谱分析方法.该方法检出限在0.03～2.13 ng/cig.之间,加标平均回收率在92.6%～110.4%之间,相对标准偏差在0.18%～6.4%之间.已用该方法测定了某品牌卷烟烟气总粒相物中14种芳香胺.     

GC/MS测定锅巴中丙烯酰胺含量

建立了一种测定市售锅巴中的丙烯酰胺含量的方法.该法样品前处理不必经过溴化衍生,样品脱脂后用水提取丙烯酰胺,提取液过活性炭柱,再用乙酸乙酯将活性炭柱中吸附的丙烯酰胺洗脱.洗脱液浓缩后经气相色谱-质谱(GC-MS)定量分析,检测限为0.06 mg/kg,适合测定市售锅巴中的丙烯酰胺的含量.还考察了丙烯酰胺在水的固液两相中的分配比.     

气相色谱-质谱法测定卷烟烟气总粒相物中的乳酸

以三甲基氢氧化硫为甲酯化试剂,正戊醇为内标,采用CP-FFAP毛细管柱(25 m×0.15 mm i.d.×0.25μm d.f)和选择离子模式,建立了卷烟烟气总粒相物中乳酸的气相色谱-质谱分析方法。该方法的线性范围为0.285~0.0570mg/mL乳酸(r=0.9997),平均回收率为97.99%,RSD为1.58%。并用该法测定了部分卷烟烟气总粒相物中的乳酸。     

硒芳香杂环化合物的GC/MS分析

本文对合成的7种含硒芳香杂环化合物进行了GC／MS分析研究。结果表明：BS、MB、BBS和DBBS等4个化合物在色谱柱内的保留时间与它们的相对分子质量呈线性关系。所有化合物均可获得特征质谱,表现出含单个硒原子的分子离子或碎片离子特征峰簇,硒的两种主要同位素在峰簇中表现为主要峰M与（M-2）的相对丰度比约为2：1,可为鉴定含硒分子离子或碎片离子提供重要信息。新化合物1,2,5-硒二唑并[3,4-d]嘧啶-5,7-（4H,6H）二酮（SPDO）在色谱柱内出现11．83min和7．96min两个具有相同的质谱的色谱峰,被认为是互变异构体的峰。     

Detection of PAH of molecular weight between 300 and 402 in airborne particulate matter by fused silica capillary GC and GC/MS

Gas chromatography (GC), low-voltage mass spectrometry (LV MS), and gas chromatography/mass spectrometry (GC/MS) have been used for detecting polycyclic aromatic hydrocarbons (PAH) of molecular weight between 300 and 402 in airborne particulate matter. Nearly 200 high molecular PAH separated by fused silica capillary columns could be characterized by their El mass spectra. The lack of reference substances precluded further structure elucidation.     

GC/MS方法分析豇豆中水胺硫磷等37种农药残留

建立了GC/MS法同时测定豇豆中水胺硫磷等37种农药残留的方法.农药经过乙腈提取,NH2/CARBON复合固相萃取小柱净化,HP-5MS(30 m×0.25 mm×0.25 μm)弹性石英毛细管柱分离后,用GC/MS选择离子模式进行测定.农药在0.020～0.500 mg/L时与峰面积有良好的线性关系(r2>0.990...     

Use of small diameter WCOT columns for ultra-high resolution GC/MS

For clinical and environmental analyses utilizing capillary gas chromatography/mass spectrometry (GC/MS), increased sensitivity and speed of analysis are highly desirable. These performance advantages are realized using a WCOT column of 100 μm i.d. as compared to the more conventional 200 μm i.d. capillary columns. The improved sensitivity of capillary direct GC/MS with the 100 μm i.d. column for the confirmation of drugs of abuse will be demonstrated. For environmental analysis, the superior efficiency and resolution of the 100 μm i.d. column can be employed for the separation of priority pollutants. This approach is more amenable to capillary direct GC/MS providing a more effective interface to the mass spectrometer. As a result improved sensitivity and a considerable decrease in analysis time is achieved over that obtained with the larger diameter environmental specialty phase columns.     

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.     

A versatile all-glass GC/MS interface for capillary columns

A new all-glass interface for GC/MS designed to fully exploit the potential of glass capillary columns is described. The system works in the open split mode and has high versatility with respect to column changing. It is especially suitable for mass spectrometers, which are not exclusively dedicated to GC/MS work. Two chromatograms illustrate the properties of the described interface.     

对2008年一道高考化学题的实验研究——是对甲基苯酚还是邻甲基苯酚

2008年一道高考化学题曾引起过不小的争论。争论的焦点是,一种甲基苯酚,与溴水反应生成的一溴代物只有2种,它应该是对甲基苯酚还是邻甲基苯酚?为了解决上述问题,用GC/MS法进行了实验研究。结果表明：对甲基苯酚与溴水反应生成的一溴代物只能观察到1种,而邻甲基苯酚与溴水反应生成的一溴代物则能观察到2种,二者均未观察到生成羟基间位溴代产物。由此可得出结论,该化合物应该是邻甲基苯酚。