系列新型咔哚聚芳醚砜结构的裂解色谱—质谱研究

利用裂解色谱－质谱对４个同一系列新型咔哚聚芳醚砜样品的裂解规律进行了研究，分别得到了各自链节的裂解特征碎片，证明了各聚合物确实发生了缩聚反应。     

Pyrolysis gas chromatography-mass spectrometry of natural resins used for artistic objects

Summary Eight resins used as protective layers for paintings, small sculptures, jewelries and artistic furniture, namely, Manila copal, colophony, Venice turpentine, elemi, shellac, dammar, sandarac and mastic were subjected to pyrolysis gas chromatography-mass spectrometry (PY-GC-MS). Significant mass spectral ions were monitored in each pyrogram. A table for identification of such resins based on the most significant ions in the mass spectra of the pyrolysis fragments is proposed. The results of PY-GC-MS analysis of a sample from the earth globe Giovanni Enriques, attributed to the Venetian geographer Vincenzo Coronelli (1650–1718) (Museo della Specola, Department of Astronomy, University of Bologna), are reported as an example of practical application of the method to a real artistic sample.     

喷气燃料中胶质化合物的质谱分析

喷气燃料中的不安定组分对燃料安定性影响很大,不安定组分主要集中在胶质化合物中,胶质化合物的存在会增加燃烧积炭,影响航空发动机的正常使用[1-2]。不安定组分含量极少,必须通过一定条件的分离和富集才能进行分析和评价。本文采用中性氧化铝吸附和极性溶剂脱附的方法分离制备     

白酒中游离有机酸的定量测定

本文介绍了一种简单、准确测定白酒中游离有机酸的方法。酒样经中和、浓缩后,未经衍生直接注入毛细管色谱柱,经气相色谱-质谱鉴定并采用三种内标物定量,可准确测定白酒中C2～C18的二十种游离脂肪酸及三种苯羧酸,结果重现性良好。     

聚芳醚酮（砜）亚胺的裂解色谱质谱鉴定

本文通过对聚芳醚酮亚胺和聚芳醚砜亚胺两类聚合物的裂解色谱质谱的解析,归纳出适合于正确鉴定这两类新型聚合物的表征化合物。     

气相色谱-质谱法测定玩具中的9种有机物残留量

建立了气相色谱-质谱测定塑料玩具中乙二醇单乙醚、2-甲氧基乙酸乙酯、苯乙烯、2-乙氧基乙酸乙酯、环己酮、双(2-甲氧基乙基)醚、三甲苯、硝基苯、异佛尔酮9种有机物残留量的方法.不同材质的塑料玩具样品经相应溶剂提取,离心后的澄清溶液经Envi-carb石墨化碳固相萃取小柱净化,旋蒸、氮吹浓缩,甲醇定容,过0.2 μm滤膜...     

GC/MS Identification of Organic Pollutants in the Caroni River,Trinidad

Abstract

Water samples from the Caroni River, Trinidad and other rivers which flow into the Caroni River were qualitatively analyzed for trace organic contaminants by procedures based on XAD extraction followed by GC/MS analysis. Pesticides, polyaromatic hydrocarbons, aliphatic hydrocarbons, phenols and phthalate esters were the main groups of compounds found. Many of the contaminants present in these water samples are known industrial pollutants, and several have been found in waste waters examined by other workers, which suggests that the factories of an industrial complex located upstream of the Caroni/Arena Water Treatment Plant may be the major source of the pollutants. Some compounds identified in the water samples have not been previously reported.     

顶空气相色谱-质谱法测定玩具中10种有机物的迁移量

建立了顶空气相色谱-质谱测定玩具中10种有机物迁移量的方法.样品在30mL去离子水中迁移60 min,得到的迁移液经95℃、90 min静态顶空后,通过60 m DB-624色谱柱分离,质谱进行检测,外标法定量.方法对于不同有机物的定量限(LOQ)在16.7～83.3μtg/L之间,线性范围为0.0167～16.7 m...     

顶空固相微萃取–气相色谱–质谱法检测絮用纤维中有机挥发物

采用顶空固相微萃取–气相色谱–质谱联用法测定絮用纤维中甲苯、乙烯基环己烯、1,3-丁二烯等29种常见有机挥发物的含量。样品在120℃平衡20 min,然后固相微萃取30 min,在250℃的进样口温度下解吸10min。29种有机挥发物在检测范围内均有良好的线性,线性相关系数r≥0.99,检出限为0.000 5~0.016 mg/m~2。3个添加标水平下平均加标回收率为88.4%~113.4%,测量结果的相对标准偏差小于11%(n=6)。方法快速、灵敏,适用于絮用纤维中有机挥发物快速检测。     

卷烟搭口胶的裂解气相色谱-质谱分析

卷烟搭口胶是用在卷烟制造过程中必不可少的辅助材料,由于它直接参与烟支燃烧,因此对卷烟的产品质量和生物安全具有较大的影响.     

顶空/气相色谱-质谱法同时测定报纸中14种溶剂残留

建立了同时测定报纸中14种溶剂残留量的顶空/气相色谱-质谱分析法。采用顶空气相色谱技术,以毛细管柱(Agilent HP-INNOWAX,60 m×250μm,0.25μm)分离,选择离子监测模式(SIM)下进行质谱检测。在优化的顶空/气相色谱-质谱分析条件下,14种溶剂残留在2~20μg范围内线性关系良好,相关系数均不小于0.995;方法的定量下限(S/N=10)均小于0.01 mg/m2。加标水平为3.97~16.28μg时,待测物的平均回收率为86.6%~101.8%,相对标准偏差(RSD,n=6)均不高于6.8%。本方法快速、准确、灵敏,适用于报纸中溶剂残留的测定。     

密闭环境中人体自身代谢挥发性有机化合物气相色谱/质谱分析

参考EPA TO－14方法,以稍加改装热解析装置Tekmar6000和吹扫捕集装置Tekmar 3000作为进样系统,对密闭环境中人体挥发性有机化合物（VOCs)进行了GC／MS定性分析和外标定量,初步确定了密闭环境中的生活人员给密闭的生活环境带来的污染成分,为密闭环境的气体净化提供了依据。     

Identification of Organic Volatile Markers Associated with Aroma during Maturation of Strawberry Fruits

In the present study, organic volatile markers of three strawberry varieties (Albion, Festival and Frontera) during the maturation process were investigated. Forty metabolites associated with aroma in fresh strawberries were monitored during seven stages of maturation using gas chromatography–mass spectrometry (GC-MS) equipped with headspace-solid phase microextraction (HS-SPME). The data were evaluated using multivariate analysis to observe correlations between the organic volatile compound profile and the seven phenological stages of maturation for each strawberry variety. The dynamic levels of butanoic acid methyl ester, hexanoic acid methyl ester, octylcyclohexane, cyclohexane,1,1,2-trimethyl, linalool, tetradecane, and α-muurolene underwent distinctive changes in concentration during the maturation process. The multivariate analysis also allowed the identification of these compounds as possible volatile markers to measure the maturation of strawberry fruits in all three varieties. These findings highlight the importance of the timing of harvest and maturation stage in each variety to preserve or improve the desirable aromatic characteristics of strawberry fruits.     

体液中-叶萩碱检测方法的研究

本文报道了用气相色谱(GC)及气相色谱-质谱联用(GC/MS)检出人体液中一叶萩碱的方法.尿样经碱化后用乙醚直接萃取,回收率为72.1％;血浆样品用Sep-pak小柱提取,回收率为 43.9％,GC/MS的检测限为 20ng.方法快速、简便、准确.     

顶空气相色谱-质谱法测定涂料中的5种挥发性有机物

建立了涂料中5种挥发性有机物(VOCs)的顶空气相色谱-质谱(HS/GC-MS)分析方法.对溶剂、平衡温度、平衡时间、GC-MS的分离检测等实验条件进行了优化.涂料样品经N,N-二甲基甲酰胺(DMF)-水(1 :1,体积比)溶解分散,经90 ℃、90 min静态顶空后,通过DB-VRX色谱柱分离和质谱检测,外标法定量....     

顶空气相色谱-质谱测定橄榄调和油中橄榄油含量

建立了测定橄榄调和油中橄榄油含量的顶空气相色谱-质谱分析方法。对样品量、加热温度、加热时间、进样量、进样模式、色谱柱进行了优化。通过化学计量学方法发现了橄榄油的特征化合物。取1.0 g样品放置于20 m L顶空瓶中,在180℃加热振摇2 700 s,取1.0 m L顶空气体进样,通过HP-88色谱柱分离和质谱检测。结果表明,方法的线性范围为0~100%(橄榄油含量),线性相关系数(r2)大于0.995,检出限为1.26%~2.13%,模拟橄榄调和油中橄榄油含量测定的偏差为-0.65%~1.02%,相对偏差为-1.3%~6.8%,相对标准偏差为1.18%~4.26%(n=6)。该方法不使用任何溶剂,操作简单、快速、环保,灵敏度和准确度高,适用于橄榄调和油中橄榄油含量的测定。     

成都地区雨水中有机污染物成份的研究

本文采用自行研制的雨水富集提取器吸附富集雨样中复杂有机物，不需预分离，直接用于ＧＣ和ＧＣ／ＭＳ分析。鉴定出１０２种有机物，并对ＢａＰ等２８种主要污染物作了定量测定。     

Chromatography-mass spectrometry and toxicity evaluation of selected contaminants in seawater

Summary In the present work a combined analytical study involving gas and liquid-chromatography and toxicity studies were developed for the determination of various contaminants typically present in sea water samples. The compounds investigated were Diuron, Chlorothalonil, Dichlofluanid, TCMTB (2-thiocyanomethylthiobenzothiazole), lrgarol 1051, Sea nine 211 and MTBE (methyl-tert-butyl ether). The selected compounds are additives of boat paints and gasoline and they can release into the aquatic environment in considerable amounts in areas with intense shipping traffic. The developed analytical protocol consisted on the use of a solid phase extraction procedure with Oasis^™ HLB cartridges followed by GC-El/NCI-MS and LC-ES-MS both in SIM mode. Average recoveries, loading 600 mL of samples with pH=3, varied from 40 to 95% and the detection limits ranged from 1–25 ng L⁻¹. The developed method was applied to real samples from various marinas of Andalusia (Spain).Daphnia magna, Vibrio fischeri andSelenastrum capricornotum toxicity bioassays on individual and mixtures of selected compounds were applied to evaluate EC₅₀ (effective concentration) and LOEC (lowest observable effect concentration) values. Resulting values were in the range of 0.001–720 mg L⁻¹ for EC₅₀ and 0.8.10⁻⁹–30 mg L⁻¹ for LOEC for all contaminants except for MTBE where no toxic effect were found up to 680 mg L⁻¹ onDaphnia magna. Toxicity effects of binary mixtures of the selected compounds showed synergistic effects in the majority of the cases (47.6%) and antagonistic in the lower of the cases (9.5%). Levels of the contaminants found in the seawater samples showed around a 30% of inhibition on tested species, during the summer months considering mixture lrgarol 1051-Diuron. Accelerated toxicity processes were observed in mixtures MTBE-Diuron and MTBE-Dichlofluanid. Presented in the Workshop “GPoll of European Science Foundation” Barcelona, Spain, 8–10 November 2001.     

氰酸酯树脂热分解的高分辨裂解气相色谱-质谱分析

采用高分辨裂解气相色谱-质谱(HRPycC—Ms)研究了在不同裂解温度下氰酸酯树脂裂解产物分布以及主要裂解物的产率与裂解温度的关系,根据热分解产物的组成及其温度依赖性,讨论了氰酸酯树脂的热分解机理。     

松油醇的分析及其生产工艺改进的研究

 应用气相 红外光谱(GC FTIR)和气相 质谱(GC MS)对合成松油醇及其杂质成分、原料松节油、合成过程中间体粗油(红油和黄油)和天然松油醇进行了分析研究,为判断松油醇产品中杂质产生的原因及改进生产工艺提供了依据。研究结果表明,松油醇中的杂质主要为长叶烯和石竹烯,是由原料松节油带入的。天然松油醇粗油中主要成分是1,8 桉叶素、反式 4 艹守醇、p 异丙烯基甲苯、顺式 4 艹守醇、芳樟醇、樟脑、龙脑、4 松油醇、α 松油醇和黄樟素。天然松油醇中β 松油醇和γ 松油醇含量不如合成松油醇中的含量高,以此可判断松油醇是天然的还是合成的。