GC/MS characterization of mate tea leaves extracts obtained from high-pressure CO2 extraction

This work presents a study concerning the chemical characteristics and analytical separation process of the essential oil obtained from high-pressure carbon dioxide extraction of Ilex paraguariensis. The experiments were performed in a laboratory-scale unit in the temperature range of 20–40 °C, from 100 to 250 bar. A blend of the I. paraguariensis extracts was percolated through a preparative chromatographic column, containing silica gel, and successively eluted with 150 mL of each of the following solvents: hexane, toluene, dichloromethane, ethyl acetate, acetone and methanol. The raw extract and its fractions were analyzed by gas chromatography coupled to mass spectrometry detection (GC/MS). The fractionation procedure showed to be a good clean up technique due to the isolation of different classes of compounds in each fraction. Chromatographic analyses allowed the identification of caffeine, fatty acids and esters, phytol, squalene, Vitamin E, stigmasterol derivatives and saturated hydrocarbons.     

Rapid analysis of polymer homologues and additives with SFE/SFC-MS coupling

A rapid and easy analysis method for polymers is presented. The method involves sample preparation by SFE, separation of the extracted compounds by SFC and simultaneous quantitative detection by FID, as well as identification of unknowns by MS. The applications illustrate how structural research work and routine polymer analysis can be done with this time saving method.     

Natural isotope fractionation in the discrimination of sugar origins

More than 500 carbohydrate samples have been characterised by hydrogen, carbon and oxygen isotopic parameters measured on ethanol and water resulting from controlled fermentation. Different chemical states of the carbohydrate pool have been considered: polysaccharides from cereals, tubers and leguminosae (maize, sorghum, rice, wheat, barley, potato, bean), glucose, fructose and sucrose from fruits (pineapple, citrus, apple, soft fruits), sucrose from sugar plants (beet, cane). The overall carbon-13 content of ethanol and the deuterium and oxygen-18 contents of water before fermentation were determined by mass spectrometry of isotope ratios whereas the investigation of site-specific natural isotope fractionation by deuterium NMR has provided access to the deuterium contents in the methyl (I) and methylene (II) sites of ethanol. The results have been analysed in the multidimensional space of these isotopic variables. Hierarchical clustering, principal component and discriminant analyses have been performed. Among fruits, for example, the pineapple group exhibits a 100% discrimination with respect to the apple and citrus groups which are themselves well distinguished. A still higher discrimination is reached between the three groups, citrus, cane and beet, and the addition of 10% exogenous cane or beet sucrose to citrus juice is unambiguously detected.     

Effect of igneous activity on hydrocarbon source rocks in Jiyang sub-basin, eastern China

A 50 m thick diabase sill was found in the Paleogene black mudstone hydrocarbon source rocks in Xia38 well. Within heating aureola of the sill, optical changes of kerogen and signatures of extractable bitumens in the mudstones were investigated. Under effects of high heating rate associated with sill intrusion, the vitrinite reflectance (Ro) has an increasing tendency with decreasing distance to the sill both below and above the sill. However, only within a zone of about 15 m to the diabase sill, the vitrinite reflectance shows significant increase. Above the sill, the Ro values increase gradually from 0.6% to 1.0%, whereas below the sill, the Ro values increase dramatically from 0.8% to 3.8%. The contrasting Ro increasing patterns are attributed to the different heat transferring conditions, the relatively open system above the sill and the relatively close system below. The more mature signatures below the sill are also demonstrated by the n-alkane distribution, carbon predominance index and odd-to-even carbon number predominance of the extracted bitumens. Below the sill, the proportion of the saturated hydrocarbons in the extracted bitumens increases from 34% to 79% towards the sill contact. The bitumens in the two highest rank samples which are closest to the sill are dominated by saturated or saturated + aromatic hydrocarbons.The %20S, %αββ and %Ts biomarker parameters of the extracted bitumens are 46%, 58% and 54%, respectively, at Ro = 1.5%. At Ro = 2.6% or 3.0%, they reach to 52%, 71%, and 71%, respectively, still under or close to their corresponding equilibrium end-points. These samples of high rank, established on the basis of optical assessment (vitrinite reflectance), have less mature biomarker signatures. The remarkable disparities between optical and biomarker parameters can be ascribed to that the aromatization of kerogen to increase Ro was more favored than the isomerization of biomarker in the rapid heating scenario.     

将Word文档自动转换成PDF格式的编程实现

在日常工作中,人们普遍使用微软Word编辑器制作文本文档,而PDF格式文档以其平台独立性和安全性等特点备受文档管理和发布者青睐。本文介绍Word文档到PDF文档转换的手工操作方法,同时详细论述编制转换组件,建立不同应用环境下的应用程序的过程,实现MS Word格式文档向PDF格式文档的自动、批量转换。     

GC/MS法建立烟用香精指纹图谱研究

采用超声辅助液液萃取法(ULLE)对8个不同批次的烟用HMT香精成分进行提取,用GC/MS对其进行定性定量分析,建立了该香精的GC/MS指纹图谱的研究方法,目的在于为烟用香精质量控制提供一种方便、快捷、可靠的分析手段。结果表明:ULLE方法具有操作简便、快速、节能、萃取效率高、重现性好等特点,适合于烟用香精成分的提取。8个批次的HMT香精的指纹图谱稳定性好,相似度高,具有很强的特征性和唯一性。通过该香精指纹图谱的建立,对日后进厂的HMT香精进行质量控制提供了依据。     

QuEChERS-高效液相色谱串联质谱法测定甜橙中哒螨灵和螺螨酯

[目的]建立了甜橙全果、果肉、果皮、果渣、橙汁和精油等6项基质中哒螨灵和螺螨酯的QuEChERS-高效液相色谱-串联质谱分析检测方法(HPLC-MS/MS)。[方法]甜橙样品经乙腈提取,PSA、GCB、MgSO4净化,高效液相色谱-串联质谱仪配备电喷雾正离子多反应监测(MRM),外标法定量。[结果]甜橙6种基质通过此分析检测方法,哒螨灵和螺螨酯在0.001~1.25 mg/L质量浓度范围线性相关系数不小于0.9965,3个加标水平(0.01、0.5、5 mg/kg)下哒螨灵回收率为81%~93%,RSD为0.5%~6.5%,螺螨酯回收率为81%~99%,RSD为0.5%~7.9%。[结论]该方法简单、方便、灵敏度、准确度高,覆盖甜橙全项样品基质,可适用于大批量样品快速分析。     

超临界CO2萃取丁香花蕾的工艺研究及对萃取物的GC—MS分析

本文应用超临界二氧化碳技术 ,研究了丁香花蕾的最佳萃取工艺。结合温度、压力、堆积密度、CO2 流量等因素对丁香花蕾提取物的萃出率的影响 ,采用四因素三水平的正交设计 ,得出丁香花蕾油萃取的最佳工艺条件为 :压力30MPa ,温度 4 5℃ ,CO2 流量 10L/h ,低堆积密度。作者还对萃取出的丁香花蕾油进行了GC—MS成分分析     

大理地区烤烟陈化过程中有机酸含量变化研究

使用衍生化-气质联用方法研究了大理地区烤烟连续陈化4年其有机酸变化。结果表明,烤烟在陈化过程中,①非挥发酸在6到18个月内含量明显降低,18到30个月内变化减缓,30到48个月内下降又加快,非挥发酸总量与苹果酸含量线性相关;②半挥发酸随陈化时间延长呈缓慢下降趋势;③挥发酸总量在6到24个月的陈化时间内明显增加,24到36个月内保持不变并略有下降,36到48个月内基本呈下降趋势,挥发酸总量与异戊酸含量线性相关。     

产地不同的两种香蓼的挥发性成分研究

本文通过分析检索,从香蓼1#样中鉴定出33个挥发性成分,从香蓼2#样中鉴定出36个挥发性成分。1#样中主要有十二烷醛、癸醛、草蒿脑、石竹烯氧化物、十二烷醇、癸醇等。2#样中主要有十二烷醛、癸醛、十三碳烯、十二烷醇等。二者相同的化学成分有17种,主要是癸醛、十二烷醛、十二烷醇等。