固相萃取分离煤直接液化全馏分油族组成研究

煤直接液化全馏分油组成复杂,深入认识煤直接液化油化学组成时,一般要分离成饱和烃、芳烃、胶质等不同的族组分,然后再对每一组分进行详细的分析表征,固相萃取是快速、高效分离油品族组成的方法之一。根据煤直接液化全馏分油的特点,重点研究了固相萃取法分离煤直接液化油族组成时,固相萃取材料与样品重量比、饱和烃洗脱溶剂加入量、溶剂洗脱速率等对煤直接液化油中饱和烃和芳烃组分分离效果的影响,获得了最佳分离条件。     

饱和烃中正构、异构烷烃的分离方法研究

饱和烃样品是由原油或沥青A样品先经过中性层析硅胶、氧化铝吸脱附,用正己烷淋洗出来的。当饱和烃中异构烷烃含量很高时,由于柱分离效能的原因,不能完全将正、异构烷烃各组分分离。当饱和烃经过尿素络合分离后,就能将饱和烃中的正构、异构烷烃进行很好的分离开来。进而大大地提高了色谱数据的准确性。     

致敏染料的液相色谱检测方法

建立了一种液相色谱检测致敏染料的方法。采用高效液相色谱-二极管阵列检测器对甲醇溶解的染料样品中各个有机组分进行分离,用保留时间定性,峰面积外标法定量。对有检出致敏染料的样品采用液相色谱-串联质谱法进行二次定性。     

GC-MS用于测定柴油烃组成的应用

应用GC-MS测定柴油中的烃组成,通过萃取柱将柴油馏分分离成饱和烃和芳烃组分,分别进入气相色谱-质谱联用仪分析,对采集的谱图进行定性分析和定量分析,即可测定出柴油样品中烃组成。采用GB/T11132-2008荧光指示剂吸附法对同一样品进行对比分析,实验结果表明,GC-MS法与GB/T11132-2008荧光指示剂吸附法的实验结果吻合,并能给出有关柴油烃族组成的详尽分布规律。     

气相色谱法测定染料中有害溶剂含量

建立了测定染料产品中有害溶剂含量的气相色谱(外标法)检测方法。用气相色谱对样品中的有害溶剂及其他有机组分进行分离,用峰面积外标法进行定量。通过气相色谱-质谱联用仪对有害溶剂进行了定性。样品的加标回收率为90%~110%;有害溶剂检测的相对标准偏差小于1%。结果显示,该方法线性良好,回收率、精密度好,灵敏度高,符合检测要求。     

C.I.溶剂红52中对甲苯胺含量的测定

本文建立了测定C.I.溶剂红52产品中对甲苯胺含量的气相色谱(外标法)检测方法。用气相色谱对样品中的对甲苯胺及其他有机组分进行分离,用峰面积外标法进行定量。对甲苯胺的检出限为10 mg/kg,样品的加标回收率为70%~130%;对甲苯胺检测的相对标准偏差小于5%。     

气相色谱法测定染料产品中喹啉的含量

建立了测定染料产品中喹啉含量的气相色谱(外标法)检测方法。用气相色谱对样品中的喹啉及其他有机组分进行分离,用峰面积外标法进行定量。通过气相色谱-质谱联用仪对喹啉和异喹啉进行了定性。喹啉的检出限为10 mg/kg,样品的加标回收率为70%~130%;喹啉检测的相对标准偏差小于2%。结果显示,该方法线性良好,回收率、精密度好,灵敏度高,符合检测要求。     

高效微型液相色谱与高温气相色谱联合测定润滑油族组成

采用填充毛细管液相色谱 (PC -HPLC)与高温毛细管气相色谱 (CGC)在线联用技术分析润滑油全组分。PC -HPLC柱 ( 0 .32mmi.d .)用于样品族分离 (烷烃、单环芳烃、双环芳烃、三环芳烃和胶质 )。经PC -HPLC分离后的各族组分被依次存放在多位储存接口内 ,然后分别转入GC作单个族组分的定量分析。该方法是解剖进口润滑油基础油及新产品开发中强有力的分析手段。     

沧东凹陷古近系孔二段烃源岩特征评价

通过对沧东凹陷古近纪孔二段部分取样井的岩心的进行观测与取样,对沧东凹陷古近系孔二段烃源岩的地层厚度与分布特征进行分析研究;并对泥岩烃源岩样品进行有机地球化学的分析测试,其中分别包括对总有机碳(TOC)测试、镜质体反射率(R_o)测定、岩石热解分析、全岩有机显微组分分析、氯仿沥青"A"抽提、族组分分离等分析方法进行分析,完成了对沧东凹陷古近系孔二段烃源岩的有机质丰度、有机质类型以及有机质成熟度的研究,从而对沧东凹陷古近系孔二段烃源岩进行评价。研究结果表明,研究区烃源岩有机质丰度普遍较高,型以Ⅱ1、Ⅱ2为主,部分为Ⅰ型有机质,没有Ⅲ型有机质。有机碳(TOC)值为0.12%～76%,平均值为2.23%,大部分超过生烃门限(0.2%);镜质组反射率为0.627%～0.888%,总体上处于成熟阶段。     

高效微型液相色谱与高温气相色谱联合测定润滑油族组成

采用填充毛细管液相色谱（ＰＣ－ＨＰＬＣ）与高温毛细管气相色谱（ＣＧＣ）在线联用技术分析润滑全组分。ＰＣ－ＨＰＬＣ柱用于样品族分离（烷烃、单环芳烃、双环芳烃１三环芳烃与胶质）经ＰＣ－ＨＰＬＣ分离后的各族组分被依次存放在多位储存接口内,然后分别转入ＧＣ作单个族组分的定量分析。该方法是解剖进口润滑油基础油及新产品开发中强有力的分析手段。     

Investigation of a hydrothermally treated brown coal by i.r. and Chromatographic methods

I.r. spectra of a brown coal (Merseburg, GDR) and two hydrothermally treated samples, and their solvent extracts, were studied. Difference spectra showed a significant increase in the aliphatic absorptions, a decrease in hydroxy groups and changes in the carbonyl, carboxylate and carbonate group contents as a consequence of the treatment. Eight fractions of each extract separated by column chromatography were also investigated, the hydrocarbon fractions by gas chromatography and the other fractions by i.r. spectroscopy. The non-uniform distribution of n-alkanes in the original sample became uniform after the treatment.     

High Performance Liquid Chromatography–Size Exclusion Chromatography for Rapid Analysis of Total Polar Compounds in Used Frying Oils

Analysis of used frying oil samples by high performance liquid chromatography–size exclusion chromatography (HPLC–SEC or HPSEC) was compared to AOCS Official Method Cd 20-91 (silica gel column chromatography) for the purpose of developing a rapid analysis of total polar compounds (TPC). In a direct comparison of the two analytical methods using four different sets of used frying oils (21 total oil samples) ranging from fresh to discard quality (4.3 to 35.4% TPC by column chromatography), the weight percent total polar compounds (%TPC) determined by HPLC–SEC averaged 0.71% higher than the values by silica gel column chromatography. Reproducibility of the HPLC–SEC method of s _r = 0.30 and RSD_r% = 1.22 compares to the variability of s _r = 0.29 and RSD_r = 1.3 for samples of approximately the same %TPC, reported in AOCS Method Cd 20-91. Because the rapid method does not separate pure (non-polar) triacylglycerol (TAG) and polar, oxidized TAG (OX-TAG), a high concentration of OX-TAG will quantitatively affect the results. This places practical limits on the types of studies to which the method may be applied if a separate analysis for the OX-TAG is not performed. Advantages of the HPLC–SEC method include the following. It uses about 75% less solvent than standard column chromatography methods for determination of %TPC. This HPLC–SEC method is very similar to AOCS Official Method Cd 22-91, and thus, also separates and quantifies polymerized triacylglycerols. The HPLC–SEC method determines both TAG polymer concentration and %TPC of used frying oils in about 1 h.     

Ultra high performance liquid chromatography–mass spectrometric analysis of oxidized free fatty acids and acylglycerols

A fast ultra high performance liquid chromatography (UHPLC)–electrospray ionization (ESI)–mass spectrometric (MS) method was developed for simultaneous analysis of free fatty acids (FFAs), monoacylglycerols (MAG), diacylglycerols (DAG), triacylglycerols (TAG), and their oxidized equivalents. Effect of elevated column temperature was studied in order to optimize the chromatography of closely eluting peaks and to reduce high back pressure formed in UHPLC. The elevated temperature enabled high flow rate, better mass transfer, and therefore more narrow peaks and better separation of the analytes. The new method was applied to the analysis of total lipid extracts of lipolysis samples prepared by an artificial digestion model in order to investigate oxidized lipids and changes in their profiles in the chyme. Over 150 compounds were identified from the extracts. The UHPLC–ESI–MS method was proved to be fast, highly selective, and sensitive. Compared to a previously used high performance LC–ESI–MS method, the new UHPLC–ESI–MS method was over five times faster and consumed one tenth of the solvents while producing comparable quantitative results. Practical applications: Edible oils and fats contain mainly TAGs, the lipolysis of which produces FFAs and MAGs with minor DAG components. These compounds are susceptible to oxidation in the stomach, and therefore the analysis of the oxidation products is important. Fast determination of FFAs and acylglycerols is also important in quality control of biodiesel. Our new method enables accurate and sensitive determination of different molecular species present in digested and processed samples with minimal sample preparation requirements. In this respect, the new method is applicable to large scale and fast screening of biological samples for lipidomic and metabolomic studies.     

Extractable hydrocarbons and kin recognition in honeybee (Apis mellifera L.)

Hydrocarbons of worker honeybees of known pedigree were extracted and analyzed using gas chromatography and mass spectrometry. Variability in hydrocarbon extracts of individual workers is determined at least in part genetically. Correlations in hydrocarbon composition of extracts were highest among more closely related individuals. Individuals maintained in groups exchange hydrocarbons but still maintain enough self-produced compounds to retain genetically determined individual characteristics. These results demonstrate that extractable hydrocarbons of bees provide sufficiently reliable genetic information to function as labels for use during kin recognition.     

高效液相色谱—氢火焰检测器测定柴油烃族组成研究

近年来，全球性城市空气污染问题日益严重，许多国家都在研究或启动控制空气质量的项目，由于石油燃料的使用是导致大气污染的主要原因之一，因此为了使用清洁燃料而对燃料配方进行调整便是采取的一项主要措施。例如在我国主要城市，含铅汽油已被禁止使用。柴油是目前使用...     

Lipid composition of beef heart ventricle

The lipid class composition of beef heart ventricle was determined by a combination of diethylaminoethyl cellulose column chromatography and quantitative thin-layer chromatography. Percentages of the total lipid were: triglyceride, 43.6; cholesterol, 7.4; phosphatidyl choline, 22.8; phingomyelin, 4.0; phosphatidyl ethanolamine, 11.2; diphosphatidyl glycerol, 5.8; phosphatidyl serine, 1.2; phosphatidyl inositol, 3.0; phosphatidyl glycerol, 0.9; unsaturated hydrocarbon, 0.02; saturated hydrocarbon, 0.20. Nonlipid components represented 33.6% of the crude chloroform/methanol extracts.     

Hydrocarbons ofNasutitermes acajutlae and comparison of methodologies for sampling cuticular hydrocarbons of caribbean termites for taxonomic and ecological studies

Using data from the arboreal nestingNasutitermes acajutlae (Holmgren), we propose standard collection and extraction methodology for characterization of cuticular hydrocarbons of termites under field conditions in the tropics. Specifically, we evaluated: (1) the effect of the duration and the number of extractions; (2) the effect of drying termites before extraction; (3) the effect of sample size; (4) the effect of solvents (ethanol versus hexane) on cuticular hydrocarbon profiles. Olefins comprise ca. 70% of the cuticular hydrocarbons ofN. acajutlae. Hydrocarbons consist of two distinct groups: early-eluting components, primarilyn-alkanes and methyl-branched alkanes, and late-eluting compounds, which consist almost exclusively of unsaturated components with one to six double bonds. Soldiers have more early-eluting compounds than workers or alates. Nests from the same island had qualitatively similar, but quantitatively dissimilar hydrocarbon mixtures. Brief extractions of 300 live workers in 10 ml of hexane for only 20 sec produced a hydrocarbon mixture equivalent to a 10-min extraction. Long-term extraction of 300 workers in hexane for two years resulted in different mixtures of hydrocarbons. Drying workers tended to enhance extraction of the less abundant unsaturated compounds such as C_41.4 and C_41.5. A single extraction of a minimum of 100 workers (live or dried), with hexane for 20 sec to 10 min is best; these extraction regimes resulted in mixtures of hydrocarbons that are quantitatively very similar. For quantitative comparisons, extracts from dried samples should not be compared to those from live samples. Storage in ethanol caused numerous unidentified, nonhydrocarbon compounds to be extracted either from the cuticle or from internal tissues.     

新疆黑山煤液化重质油340-360℃馏分离及分析

用气相色谱/质谱联用仪(GUMS)分析馏程为340-360℃的新疆黑山煤液化重质油,检测出的主要成分为稠环芳烃及其衍生物,此外还有正构烷烃和少量含氧化合物.在超声辅助条件下,对液化重质油进行甲醇萃取,所得第一次甲醇萃取物用硅胶柱层析法分离.各洗脱馏分用GC/MS分析,其可测成分与直接检测相比更丰富,表明合适的预分离对提...     

银杏叶提取物中银杏酸的分离与分析

通过萃取、层析和固相萃取等方法预处理银杏叶处提取物，然后用HPLC制备色谱柱自制银杏酸纯品，结合紫外光谱、氢核磁共振和高效液相色谱，对银杏酸进行结构解析，结果得到银杏酸I、Ⅱ、Ⅲ3种纯化合物，这3种化合物的氢核磁共振所显示的官能团证实银杏酸类化合物；并建立了HPLC法检测银杏叶提取物中的银杏酸的方法。