碳五馏分组分的HP-1毛细管色谱法测定

提出用ＨＰ－１毛细管色谱柱分析测定碳五馏分中组分含量的分析方法,研究了其测定条件,并对分离后的组分用质谱方法进行定性,按确定的分析条件,碳五馏分中各组分得到较好的分离,精密度好,分析结果准确可靠。     

大叶桉叶挥发油的化学成分研究

用挥发油提取器提取大叶桉干叶中的挥发油,利用色质联用(GC/MS)产生的双线性数据,藉化学计量学分辨方法,得到了各组分的纯物质色谱峰和质谱图。根据色谱保留时间,同时利用解析所得的纯物质质谱图在NIST质谱数据库进行相似检索来对各个组分进行定性分析;采用色谱峰面积归一法计算各化合物的相对含量。共分离了113个化合物,鉴定了其中90个,占总挥发油的93.28%。主要为萜类、萜醇类等化合物,还成功地检测出一些色谱分离不完全和低含量的组分。     

填充毛细管液相色谱-高温毛细管气相色谱在线联用分析重油

重油的组成分析一直是个难题,它的沸点高,族组分种类多,各族内组分的异构体又极为繁多.最好的分析方法是用高效液相色谱(HPLC)做族分离,馏分收集后再用CGC分析.但HPLC的族馏分体积比CGC进样量大100倍.本文采用填充毛细管液相色谱(μHPLC)与高温毛细管气相色谱(HTGC)在线联用技术[1]分析重油.正相μHPLC将样品按族分离,μHPLC的柱效高,族分离能力强,而小的馏分体积(<100μL)可避免GC分流进样.在一次LC进样后,多位储存型联用接口将分离后的各族组分切割、存储并分别无损失转入HTGC分析,利用FID对高于C10的有机物的响应值相…     

四川产千金子挥发油的GC-MS分析

采用水蒸气蒸馏法从四川产千金子中提取挥发油,多次优化色谱条件,运用气相色谱-质谱联用技术进行分析。从中分离鉴定出49个化合物,占其挥发油总量的90.48%。千金子挥发油中除了主要的长链脂肪酸及其酯类化合物,含量较少但种类丰富的萜类化合物也得到了很好的分析和确证。     

藿香正气水挥发性成分的提取及其化学成分分析

优化了水蒸汽蒸馏法对藿香正气水中挥发性成分的提取条件,选用Rxi-5ms(30m×0.25mm,0.25μm)色谱柱,五阶程序升温由初始温度50℃升至240℃,利用气相色谱-质谱分离出78个组分,鉴定了其中的35个化合物。该法可以推广到其它酊剂中挥发性成分的提取和分析。     

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。     

高温气相色谱和高温气相色谱-质谱法对费托合成蜡的分离和鉴定

费托合成蜡是费托合成反应中的重要产物之一。采用高温气相色谱与冷柱头进样相结合的方式,建立了一种分离分析费托合成蜡的气相色谱方法。该方法无需对费托合成蜡进行预处理,使用氦气为载气,选用更长的高温色谱柱,具有平稳的色谱基线,对费托合成蜡中正构烷烃和其他未知组分有很好的分离效果,能够洗脱费托合成蜡中碳数大于C₉₀的重组分。用高温气相色谱-质谱法对费托合成蜡馏分进行定性分析,其组分有烷烃、烯烃和含氧化合物。该方法对了解费托合成蜡组分的详细信息和费托合成工艺的开发有重要意义。     

GC-MS法测定油漆行业废气化学成分及化学计量学解析

采用GU/MS法分离测定油漆行业废气污染物化学成分,利用化学计量学解析法(CRM)对重叠的色谱峰进行解析,得到各成分的纯色谱曲线和质谱,通过质谱库对解析的纯组分进行定性,用解析色谱曲线积分法进行定量.从25个色谱峰中解析出了49个组分,按检索相似度大于90%的原则,鉴定出了其中40个化合物,占总含量的92.3%.废气污染物的主要成分为苯系物和烷烃,分别占总含量的46.8%和27.2%.     

中药材中挥发油化学成分的气相色谱-质谱研究

采用水蒸汽蒸馏法从野马追花蕾中提取挥发油,用气相色谱-质谱(GC-MS)法对其化学成分进行鉴定。实验结果显示,100 g野马追花蕾中挥发油提取量为0.8 mL,可分离出49个色谱峰,对其中所含的18个组分给出了参考鉴定,约占挥发油总成分的56.34%。本法简单、快速、重现性好,适用于中药挥发油的化学成分分析。     

陈皮挥发油的气相色谱/质谱分析

用ＧＣ／ＭＳ分析复方制剂平胃散中的一种单味药材陈皮的挥发油化学成分及其相对含量,对色质联用仪产生的二维数据借助直观推导式演进特征投影法来分辨以得到组分的纯色谱和质谱,根据组分的色谱保留时间和质谱对组分进行定性,继而用总体积积分法定量。本文分离出５３个组分,其中鉴定了３４个组分,约占其挥发油总量的９６．０８％。     

OH-initiated oxidation of monoterpenes: reaction of alpha-pinene

The aim of this paper is to study the reaction products of alpha-pinene, beta-pinene, limonene, 3-carene and sabinene with OH radicals by FT-IR spectroscopy and by HPLC-MS-MS, to evaluate the secondary aerosol formation. All gas phase reaction products were quantified using reference compounds. As source of OH radicals were used H2O2 and CH3ONO. The experiments were performed at low terpene concentration (0.9-2.1 ppm) and at high terpene concentration (4.1-13.2 ppm), using H2O2 and CH3ONO as sources of OH radicals.     

Mass spectrometry analysis of terpene lactones in Ginkgo biloba

Terpene lactones are a family of compounds with unique chemical structures, first recognised in an extract of Ginkgo biloba. The discovery of terpene lactone derivatives has recently been reported in more and more plant extracts and even food products. In this study, mass spectrometric characteristics of the standard terpene lactones in Ginkgo biloba were comprehensively studied using both an ion trap and a quadrupole time-of-flight (QTOF) mass spectrometer. The mass spectral fragmentation data from both techniques was compared to obtain the mass spectrometric fragmentation pathways of the terpene lactones with high confidence. The data obtained will facilitate the analysis and identification of terpene lactones in future plant research via the fragmentation knowledge reported here.     

Composition and Antimicrobial Activity of <Emphasis Type="Italic">Helichrysum italicum</Emphasis> Essential Oil and Its Terpene and Terpenoid Fractions

The essential oil of Helichrysum italicum (Roth) G. Don from Croatia has been fractionated into terpene and terpenoid fractions and analyzed using GC/MS. Fifty-two compounds were identified. The main hydrocarbons of the oil were α-pinene (10.2%), α-cedrene (9.6%) aromadendrene (4.4%), β-caryophyllene (4.2%), and limonene (3.8%), while the main oxygen-containing compounds were neryl acetate (11.5%), 2-methylcyclohexyl pentanoate (8.3%), 2-methylcyclohexyl octanoate (4.8%), and geranyl acetate (4.7%). The essential oil and its terpene and terpenoid fractions were evaluated for antibacterial and antifungal activities. The screening of antimicrobial activity was conducted by a disc diffusion test and the minimum inhibitory concentration was determined against Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, and Candida albicans. The essential oil and its terpenoid fraction exhibited higher antimicrobial activity with respect to the terpene fraction. The antimicrobial activities of the oil and its terpenoid fraction were more pronounced against Staphylococcus aureus and Candida albicans.__________Published in Khimiya Prirodnykh Soedinenii, No. 1, pp. 29–32, January–February, 2005.     

Studies on the constituents of the leaves of Baccharis dracunculifolia (Asteraceae) and their cytotoxic activity

A new sesquiterpene, named baccharisketone (1), and a new monoterpene, p-methoxythymol acetate (2), were isolated from the leaves of Baccharis dracunculifolia along with seventeen known compounds (3-19). The structures of the new compounds were determined by spectroscopic means. The growth inhibitory activity of the isolated compounds against leukemia cells (L 1210) was tested and three terpene phenols (4, 6, 17) and five sesquiterpene alcohols (8, 10, 11, 13, 16) were found to exhibit strong cytotoxic activity.     

Potential of solid phase microextraction and gas chromatography for quarantine-required detection of wood packaging in shipping containers

Solid phase microextraction (SPME) coupled with gas chromatography (GC) was used to detect terpene hydrocarbons inside shipping containers entering New Zealand. The utility of this system for the rapid detection of undeclared wood packaging for quarantine purposes was demonstrated. A portable dynamic air-sampling device was built to house a SPME fibre and allow the air from shipping containers to be sampled. The effects of sample flow rate and sampling time were investigated and sampling conditions of 100 mL/min for 30 s were chosen to keep sampling within the linear range. A CV of less than 15% (n = 12) was obtained for all the compounds analysed under these conditions. To obtain an estimate for the limit of detection (LOD) for the terpene hydrocarbons of interest, small quantities of lime oil were placed in an empty shipping container and the air inside was analysed. LOD (S/N = 3) was estimated to be in the order of 50-100 ng/L of air using GC with flame ionisation detection (GC-FID). Finally, the device was tested in fully laden containers and was shown to be effective for trapping terpene hydrocarbons indicative of wood packaging.     

Sesquiterpene Cyclizations inside the Hexameric Resorcinarene Capsule: Total Synthesis of δ‐Selinene and Mechanistic Studies

The synthesis of terpene natural products remains a challenging task due to the enormous structural diversity in this class of compounds. Synthetic catalysts are unable to reproduce the tail‐to‐head terpene cyclization of cyclase enzymes, which create this diversity from just a few simple linear terpene substrates. Recently, supramolecular structures have emerged as promising enzyme mimetics. In the present study, the hexameric resorcinarene capsule was utilized as an artificial cyclase to catalyze the cyclization of sesquiterpenes. With the cyclization reaction as the key step, the first total synthesis of the sesquiterpene natural product δ‐selinene was achieved. This represents the first total synthesis of a sesquiterpene natural product that is based on the cyclization of a linear terpene precursor inside a supramolecular catalyst. To elucidate the reaction mechanism, detailed kinetic studies and kinetic isotope measurements were performed. Surprisingly, the obtained kinetic data indicated that a rate‐limiting encapsulation step is operational in the cyclization of sesquiterpenes.     

薏苡仁挥发性成份的分析

本文应用同时蒸馏－萃取装置提取了薏苡仁的挥发物质，用ＧＣ／ＭＳ方法分离鉴定了５５种成份，其中主要成份为醇类（１４．１％）、醛类（９．８５％）、酮类（３．０７％）、酸类（５．９６％）、酯类（２．７４％）、烃与萜类（５０．４３％）、杂环类（１２．４５％），占总挥发物质的９８．６％。     

New chiral ligands from myrtenal and caryophyllene for asymmetric oxydation of sulfides catalyzed by metal complexes

From myrtenal and caryophyllene, widespread terpene compounds, three new chiral Schiff bases were prepared suitable for ligands in vanadium ions catalyzed sulfides oxidation to chiral sulfoxides.     

Study of natural coumarins by mass spectroscopy

Conclusions The mass spectra of six compounds have been obtained: kamolone, kamolol, [D₃]kamolone, [D]kamolol, kamolol acetate, and the terpene diol derived from kamolol. The fragmentation of these compounds under the action of electron impact have been discussed. The mass spectra of kamolone and kamolol agree well with the structures provided for them previously.Khimiya Prirodnykh Soedinenii, Vol. 6, No. 3, pp. 296–300, 1970