气相色谱-质谱法分析木奶果挥发油的化学成分

采用水蒸汽蒸馏法从大戟科木奶果中提取挥发油,用气相色谱-质谱对挥发油的化学成分进行了分析。鉴定出19种化合物,占总油量的100%,用面积归一化法测定了各成分的相对百分含量。木奶果挥发油主要成分为正十六碳酸、丁基甲氧基苯、9,12-十八碳二烯酸,分别占挥发油总量的29.53%、17.47%和11.59%,三者占其总量的58.59%。     

Isotope dilution determination of polycyclic aromatic hydrocarbons in olive pomace oil by gas chromatography-mass spectrometry

A gas chromatographic (GC) method with mass spectrometry detection (MS) for the determination of eight polycyclic aromatic hydrocarbons (PAHs) in olive pomace oil has been developed. The oil was diluted with n-pentane and extracted by liquid-liquid partition with dimethyl sulphoxide (DMSO). After water addition and back-extraction with cyclohexane, a thin-layer chromatography on silica gel was performed as a further purification step. The PAHs spot was scraped off from the plate and the final extract was concentrated and analysed by GC-MS in full scan mode. The eight PAHs under investigation were determined in the presence of the corresponding labelled compounds added as internal standards to the sample at the beginning of the analytical process. The identified PAHs were then quantified by the isotope dilution methodology assuring the compensation of the concentration of each analyte for any variation in the sample preparation. The method precision was satisfactory with relative standard deviation (R.S.D.) values in the range 3.6-12.7% for all PAHs. The average recovery rates ranged from 69.0 to 97.5%. Accuracy was also calculated for benzo[k]fluoranthene, benzo[a]pyrene, indeno[1,2,3-cd]pyrene and benzo[ghi]perylene by analysing a certified reference material (CRM 458, coconut oil) with adequate results. All response curves exhibited a linear fit from 0.1 to 10 microg ml(-1) and the determination coefficients R2 were better than 0.9942. The limits of detection (0.1-0.4 microg kg(-1)) were acceptable when compared with the maximum permitted limit of 2 microg kg(-1) for each of the eight considered PAHs and 5 microg kg(-1) for the sum of the eight PAHs established by the Italian legislation. Measurement uncertainty was finally calculated identifying and quantifying the uncertainty components of the analytical process. The relative expanded uncertainties (Uc), expressed as percent values were in the range 8.5-11.4% thus appropriate for residues quantification in the range of concentrations considered in the present study.     

Migration of Ethylene Terephthalate Oligomers from Roasting Bags into Olive Oil

Summary A high-performance liquid-chromatographic method with UV detection (HPLC–UV) has been developed for quantification of ethylene terephthalate oligomers in olive oil, from which they were extracted with acetonitrile. Oligomers, from monomers (M₁) to pentamers (M₅), were jointly and/or individually identified by liquid chromatography with mass spectrometry (electron-impact mass spectrometry (EIMS) low- and high-resolution) and were quantified by HPLC–UV using an acetonitrile solution of the major oligomer (the trimer M₃) as standard. For M₃ recovery was 98.9%, the detection limit was 60 g L^–2, and method precision was 2.03% (RSD). Migration of oligomers M₁–M₅ into 50 mL olive oil sealed in each of two brands of 10 cm × 10 cm poly(ethylene terephthalate) roasting bag was evaluated under two sets of conditions that approached but remained below the limit at which the bag material became physically deformed – heating for 7 min at 850 W in a microwave oven, or for 60 min at 200 °C in a conventional oven. Total migration was approximately 2.7 mg dm^–2 under the former conditions and 3.5–4.1 mg dm^–2 under the latter.Presented at the International Symposium on Separation and Characteristics of Natural and Synthetic Macromolecules, Amsterdam, The Netherlands, February 5–7, 2003     

人参挥发油的提取和分析

应用ＧＣ－ＭＳ－ＤＳ联机分析人参挥发油是当前较好的方法，但人参挥发油的提取方法和ＧＣ－ＭＳ条件的选择明显影响人参挥发油这一复杂天然混合物的分离和鉴定。本工作严格控制提取条件，提高了挥发油收率，达０．９５％；选择最佳ＧＣ－ＭＳ条件，鉴定出７６种化合物，该法稳定重现性好。     

Synthesis of a Novel Core-shell Type Acrylic-polyurethane Hybrid Emulsion Containing Siloxane and Fluorine as well as Water and the Oil Resistances of Cured Film

Aqueous acrylic-polyurethane dispersions have become one of the major types of materials used in coating, paint and adhesive industries, because of excellent properties and environmental advantages1-5. However, some properties for cured film such as water…     

A comparison between different techniques for the isolation of rosemary essential oil

Traditional hydrodistillation (HD), supercritical fluid extraction (SFE), organic solvent extraction (SE), and water microwave assisted hydrodistillation (MAHD) techniques were compared and evaluated for their effectiveness in the isolation of rosemary essential oil. The microwave assisted hydrodistillation technique was optimized in terms of both delivered power and time duration. The extracts/distillates were analyzed by GC and GC-MS. Microwave distillation, which exploits the physical action of microwaves on plants, showed a series of advantages over the other approaches: low cost, use of water in sample pre-treatment step, greatly reduced isolation time, and attainment of high quality essential oil distillate. Moreover, the absence of environmental impact of this innovative technique was also emphasized.     

Synthesis of Molecularly Imprinted Polymer Particles by Suspension Polymerization in Silicon Oil

Molecular imprinting is a method to prepare polymers with recognition site of desired and predetermined selectivity1. Molecularly imprinted polymers (MIP) are prepared by copolymerizing functional and cross-linking monomers in the presence of a molecular …     

改进的微波辅助无溶剂法提取薄荷和陈皮中的挥发油组分

An improved solvent free microwave extraction, in which a kind of microwave absorption medium （carbonyl iron powder） was used, was applied to the extraction of essential oil from dried menthol mint and orange peel without addition of any solvent and pretreatment. It took much less time of extraction （30 min） than microwave-assisted hydrodistillation （90 min） and conventional hydrodistillation （180 min）. The kinds of chemical compositions in essential oil extracted by different methods were almost the same and such improved solvent free microwave extraction can be a feasible way in extraction of essential oil from dried plant materials.     

Chemical composition and antimicrobial activity of the essential oils of Ferula latisecta and Mozaffariania insignis from Iran

The hydrodistilled oils from the aerial parts of Ferula latisecta and Mozaffariania insignis, which is endemic to Iran, were analyzed by GC and GC/MS. (Z)-Ocimenone (32.4%), (E)-ocimenone (20.3%), and cis-pinocarvone (11.4%) were the main components among the 22 constituents characterized in the oil of F. latisecta, representing 87.7% of the total components detected. Twenty-five compounds were identified in the oil of M. insignis, representing 99.0% of the total oil, with octyl acetate (41.1%), β-pinene (30.3%), and α-pinene (23.9%) as the main constituents. The essential oils were examined for their potential antimicrobial activities. Published in Khimiya Prirodnykh Soedinenii, No. 6, pp. 561–563, November–December, 2006.     

Application of Cyclodextrins to the Extraction of Antioxidant Compounds from Olive Oil

Olive oil contains powerful antioxidant compounds which impart stability, contribute to various properties of it, and are valuable from the nutritional point of view. Their extraction with as mild conditions as possible led to its investigation using cyclodextrins as a tool. The inclusion ability of α-, β-, and γ-CD was estimated, and it has been demonstrated that the small cavity of α-CD as well as the wide one of γ-CD could enclose less effectively the antioxidant compounds of olive oil than the intermediate in shape cavity of β-CD. The highest yields of antioxidant compounds were achieved when olive oil was mixed with a 2%aqueous solution of β-CD and the resulting precipitate was treated with ethyl alcohol.__________Published in Khimiya Prirodnykh Soedinenii, No. 1, pp. 18–21, January–February, 2005.