酚醛树脂的热裂解气相色谱-质谱联用分析

利用热裂解气相色谱-质谱法对两种酚醛树脂样品进行研究,选择在575℃条件下进行裂解,其裂解产物通过DB-35石英毛细管柱分离和质谱鉴定,获得了有关这两种酚醛树脂各自结构的特征信息,酚醛树脂的热裂解产物的总离子流图可认为是他们各自结构特征指纹。

气质联用(GC/MS)分析茅台王子酒的香气成分

以低度酱香型白酒—茅台王子酒为样品 ,采用气相色谱—质谱联用技术直接进样分析了茅台王子酒的香气成分 ,共分离出 2 6个色谱峰 ,并鉴定了其中 2 2个成分 ,占其香气成分的 99 17%。

蒲公英不同部位抑菌作用及代谢物差异的UPLC-MS/MS分析

为了研究蒲公英不同部位抑菌作用和代谢物成分的差异,本物采用打孔法和超高效液相色谱串联质谱(UPLC-MS/MS)方法,研究了蒲公英根、茎叶和花的水提取物和醇提取物对5种致病菌的抑菌作用,并对不同部位的代谢物成分进行了定性和定量分析。结果表明,蒲公英不同部位初提取物对变形杆菌、嗜根考克氏菌和枯草芽孢杆菌均有抑菌作用,而对大肠杆菌和铜绿假单胞菌均无抑菌作用;醇提法的抑菌效果优于水提法,花提取物的抑菌活性最强,根最弱。蒲公英的不同部位共鉴定出449种代谢物,根、茎叶和花中相对含量最高的物质分别为反油酸(脂类)、γ-亚麻酸(脂类)和木犀草素(黄酮类);且根、茎叶和花中相对含量排名前20的物质中黄酮类分别有0种、3种和8种,表明黄酮类物质可能是蒲公英中的主要抑菌活性物质。正交偏最小二乘法-判别分析(OPLS-DA)结果显示,木犀草素-7-O-葡萄糖苷在花中上调幅度最大,橙皮素C-丙二酰己糖苷为根中特有物质。本研究结果为利用蒲公英不同部位研制和开发新型药物提供了理论依据。

3-氧代硫解酶缺乏症1例报告及其尿中异常代谢产物的尿有机酸分析

目的:报告用气相色谱-质谱联用技术尿有机酸分析(GC-MS)诊断的3-氧代硫解酶缺乏症1例。方法:留取患儿尿液使用尿素酶处理标本,,再进行气相色谱/质谱分析。结果:尿有机酸分析结果显示3-氧代硫解酶缺乏症的特征性产物:大量3-羟基丁酸、2-甲基-3-羟基丁酸,中量乳酸、甲基巴豆酰甘氨酸。结论:采用尿气相色谱/质谱技术,对有机酸尿症可以进行快速诊断,并且准确性、敏感性高。

大花蕙兰鲜花香气成分的研究

利用气相色谱-质谱(GC/MS)分析技术对浙江栽培的大花蕙兰品种‘绿翡翠’(Cymbidium Hybrids)和‘台北小姐’(C.Miss Taipei)的鲜花进行了香气成分和含量的测定。结果表明:两种大花蕙兰香气成分的组成和含量存在明显差异,‘绿翡翠’的香气组成成分有43种,相对含量为97.13%,而‘台北小姐’有74种,相对含量为73.76%。两种大花蕙兰含有极少相同的化合物成分,相同成分4-甲基苯酚均为2个品种香气组分中含量最高的化合物,它与丙基环丙烷的总相对含量为53.97%,构成‘绿翡翠’的主要香气成分;与2-乙基丁醛和正己烷等23种化合物的总相对含量为55.15%,共同构成‘台北小姐’的主要香气成分。

Thermal oxidation of two aviation synthetic lubricant base oils

The thermal degradation of two synthetic lubricants base oils, poly-a-olefins （PAO） and di-esters （DE）, was investigated under oxidative pyrolysis condition and their properties were characterized in simulated ＂areo-engine＂ by comparing the thermal stability and identifying the products of thermal decomposition as a function of exposure temperature. The characterization of the products were performed by means of Fourier transform infrared spectrometry （FTIR）, gas chromatography/mass spectrometry （GC/MS） and viscosity experiments. The results show that PAO has the lower thermal stability, being degraded at 200℃ different from 300 ℃ for DE. Several by-products are identified during the thermal degradation of two lubricant base oils. The majority of PAO products consist of alkenes and olefins, while more oxygen-contained organic compounds are detected in DE samples based on GC/MS analysis. The related reaction mechanisms are discussed based on the experimental results.

新生儿型肉碱棕榈酰转移酶Ⅱ缺乏症3例尸检及文献复习

目的 探讨新生儿型肉碱棕榈酰转移酶Ⅱ缺乏症的临床及病理特征.方法 分析新生儿型肉碱棕榈酰转移酶Ⅱ缺乏症的临床表现、病理改变及串联质谱（MS-MS）分析检测,并复习相关文献.结果 尸检发现新生儿除肌肉出现大量脂肪滴之外,其他全身各个重要脏器心、肝、脾、肾等均有不同程度的脂肪空泡沉积.串联质谱（MS-MS）分析检测报告均符合肉碱棕榈酰转移酶Ⅱ缺乏症检测指标改变.结论 新生儿型肉碱棕榈酰转移酶Ⅱ缺乏症病情危重,为全身系统性疾病;诊断本疾病需结合临床、病理及实验室等各项检查.

Analysis of Volatile Constituents in Bamboo Leaves Using HS-GC/MS

[Objective] This study aimed to analyze the volatile constituents in bamboo leaves. [Method] The volatile compositions in bamboo leaves were analyzed by headspace-gas chromatography-mass spectrometry （HS-GC/MS）, and identified by searching their mass spectra in NIST database. The relative percentages of them were calculated by the GC peak areas. [Result] Fifty-three chemical constituents in bamboo leaves were separated. Among them, the main components were alcohols, ketones and aldehydes, and these compounds contained unsaturated bonds. [Con- clusion] HS-GC/MS was simple and less sample-demanding and can be used for rapid analysis of volatile constituents in bamboo leaves and provide scientific basis for further research and development of bamboo leaves.

Sex Pheromone Components of the Female Black Cutworm Moth in China: Identification and Field Trials

The sex pheromone blend of a China strain of the black cutworm moth Agrotis ypsilon （Rottemberg） （Lepidoptera： Noctuidae） was investigated. Chemical analysis of pheromone gland extracts of 3-day-old females showed that individual isolated glands contained only very small amounts of pheromone. The high-resolution gas chromatography combined with mass spectrometry （GC-MS） analysis showed the presence of Cis-7-dodecenyl acetate （Z7-12：Ac, A）, Cis-9-tetradecenyl acetate （Z9-14：Ac, B）, Cis- 11-hexadecenyl acetate （Z 11 - 16 ：Ac, C）, Cis-8-dodecenyl acetate （Z8-12：Ac, E） and Cis-5-decenyl acetate （Z5-10：Ac, D） in biologically active pheromone gland extracts. An extract of one gland from a day 3 female gave the following values for the gland components： 0.245±0.098ng for Z7-12：Ac, 0.080±0.031ng for Z9-14：Ac, 0.089±0.033ng for Z11-16：Ac, 0.085±0.031ng for Z5-10：Ac, 0.105±0.065ng for Z8-12：Ac per female. The percentages of Z7-12：Ac, Z9-14：Ac, Z11-16：Ac, Z5-10：Ac and ZS-12：Ac in pheromone gland extracts from individual females were （meaniSE） 40.451±13.66, 13.176±5.279, 14.943±5.142, 14.392±6.10 and 17.225±9.792 respectively, and the percentages of Z7-12：Ac, Z9-14：Ac and Z11-16：Ac were 58.75±9.429, 18.91±7.539 and 22.34±7.209. Field trials indicated that each single component of sex pheromone was non-effective and captured no males. The lures baited with duality compound of AB （3 ： 1） had a certain attraction to males, the mean captured number was 2.6. The attraction ability of the lures baited with ternary compound of ABC （3 ： 1 ：1） to males added significantly, the mean captured number per trap was 7.40, which was 2.8 times of duality compound of AB （3 ： 1）. The contents of sex pheromone could obviously affect its capture ability to males, the mean captured number was the highest at the dosage of 200 μg.

Microwave-assisted extraction of Shenfu coal and its macromolecule structure

Coals consist of some molecules trapped within an organic matrix from which some organic compounds can be extracted by solvents. The Soxhlet technique has been widely used for extracting organic compounds. Microwave heating methods may be successfully applied in the field of coal science. Acetone extraction yields and the chemical composition of the extract were investigated using a typical Chinese coal, Shenfu coal, with microwave-assisted extraction. The acetone extract and residue were analyzed by GC/MS and carbon-13 nuclear magnetic resonance spectroscopy respectively. The carbon spectra were converted into several numerical parameters, fa, Ha, Xb, which indicate the difference in macromolecular structure between Shenfu coal and its residue. Furthermore, a hybrid genetic algorithm was employed using these parameters to approximate a coal macromolecule by assembling the structural fragments or functional groups into a large and complicated structure.

GC/MS Analysis of Organic Compounds in Hot Water-Extractable Fraction from Shenfu Coal

Shenfu Coal was extracted with hot pure water and slurry was isolated. The concentrated benzene-soluble fraction (CBSF) was analyzed with GC/MS and four types of organic compounds (OCs) were detected: HACOCs,DTEs,DMDT and LCAs. The amount of benzyl benzoate which is the most abundant OC was calculated by an inter-nal standard method with an indicated amount of BP. The broken hydrogen bonds and ether bonds were responsible for the extraction of OCs from the coal .DTEs,DMDT and LCAs are essentially insoluble in water,whereas they are soluble,probably owing to intermolecular interaction of OCs with HACOCs.

Analysis of the major components of root exudates released from several economic forest tree using GC-MS

In 2000 and 2001, 1-year-old seedlings of 7 economic tree species including chestnut, apricot, persimmon, peach, walnut, pear and apple were cultured in garden pots that had a diameter of 40 cm and were filled with clean sand. The major components of exudates released from their roots were isolated and analysed by GC-MS. Totally 200 kinds of organic chemicals were isolated, of which 3 kinds i.e. naphthalene, dimethylbenzene and dibutyl phthalate were principally controlled pollutants according to 'Blacklist of Principal Environment Pollutants in China' and the standard of U.S. Environmental Protection Agency (EPA). The research result provided theoretical evidence for selecting low-pollution economic forest crops in the water source protection area in Miyun Reservoir.

Study on microwave-assisted extraction of coal

The effect of different factors on coal extraction yield-temperature, solvent, coal type and irradiation time were investigated for different China coals under microwave-assisted extraction（MAE）. The results show that the optimum temperature for ethanol, acetone and THF are 393,373 and 373 K respectively and the extraction yield of THF is higher than that of other two solvents under MAE. Extraction with several single organic solvents were conducted for the 5 typical China coals-Shenfu, Tongchuan, Panzhihua, Yitai and Huating coal under microwave-assisted extraction and Soxhlet extraction. Results indicat that extraction yield of ethylenediamine, ethanol, acetone, tetrahydrofuran under MAE are all higher than that of Soxhlet extraction and MAE required less time. Tongchuan coal extracts of ethanol and acetone which were extracted by MAE and Soxhlet extraction were analyzed by GC/MS.

Preparation and Evaluation of Microcapsule Containing Volatile Oil of Herba Schizonepetae by Emulsion Solvent Diffusion Method

Microcapsules of volatile oil containing Herba Schizonepetae(VOHS) were prepared by emulsion solvent diffusion method to improve the drug loading and reduce the amount of pharmaceutical excipients.Orthogonal assay was applied to optimize the preparation condition of microcapsulation,and the results illustrated that the ratio of ethyl cellulose(EC) to VOHS influenced the property of VOHS microcapsule significantly.GC-MS analysis indicated that some volatile components with low concentration in VOHS were lost after microencapsulation.The microcapsules prepared with optimum condition had good fluidity,and the holes on the surface of the microcapsules contributed to the release of VOHS.The particles of the microcapsule conformed to a normal distribution with the diameter of 45—220 μm.In the simulated intestinal fluid containing 0.2% sodium dodecyl sulfate,pulegone in VOHS microcapsule showed a certain degree of slow release.Compared with β-cyclodextrin method,the microencapsulation used in the present work could reduce the amount of excipients and increase the drug loading.It was beneficial to reduce the dose of Chinese medicines containing volatile oils.

Component Analysis of Volatile Oil of Garlic from Different Districts and Assay of Allicin Content

[ Objective] The aim was to study the chemical component of volatile oil of garlic in different districts. [ Method] GC-MS was used to an- alyze the composition of the garlic volatile oil in Guiyang, Guizhou Majiang, Shandong, Yunnan and Chongqing and the HPLC method was used to assay the content of gadicin. [ Result]Gadicin in different essential oil had the highest content but varied a lot. The sampling amount of garlicin be- tween 0.562 and 2.810 μg was in a good linear relation （R =0.999 2, n = 5 ） with peak area, the average recovery rate was 99.39, RSD = 1.76%. [ Conclusion] GC-MS can be used to analysis the composition of essential oil quickly and effectively. The liquid chromatographic analysis of garlicin was simple, reliable and reproducible. The study provided the theoretical basis for selecting garlic in gadic flavor oil production and improving quality of gadicin oil.

Maillard Products Formed from Chicken Fat Oxidants and Amino Acids Act as a Flavor Enhancer in Comminuted Chicken Products

Lipid oxidation and degradation are generally recognized as unfavorable reactions in food processing. However, lipids can be utilized to produce meat-like flavorings through reaction with amino acids after degradation to carbonyls such as aldehydes and ketones. The fatty acids in chicken fat mainly comprise palmitic acid, oleic acid and linoleic acid. After being heated at 120 ~C for 3 h, the degraded carbonyls of chicken fat were reacted with cysteine, alanine, glycine and thiamine to form a chicken-like flavoring. The key aromatic components of the flavoring were identified by GC-MS. In the overall volatile profile, 22 kinds of compound were detected, among which 2-furanmethanol was formed by the Maillard reaction, 1-（2-furanyl）-ethanone by cyclization and 2,4,6-trimethyl-l,3,5-trithiane by the Strecker degradation of cysteine. Dihydro-2-methyl-3（2H）-furanone, dihydro-2-methyl- 3（2H）-thiophenone, 2-acetyl-lH-pyrroline and 4-methyl-5-thiazoleethanol were the degradation products of thiamine. The prepared chicken flavoring was added to comminuted chicken product （CCP）. GC-MS analysis and sensory evaluation showed that the flavor and odor of the CCP were greatly enhanced.

Chemical fingerprinting of Su-He-Xiang-Wan and attribution of major characteristic peaks for its quality control by GC-MS

A simple and facile gas chromatography-mass spectrometer （GC-MS） fingerprint of Su-He-Xiang-Wan （SHXW） was developed, the similarity analysis was conducted, and attribution of the major characteristic peaks was identified for SHXW quality control. GC-MS analysis was performed on a QP2010 instrument （Shimadzu, Japan） equipped with a capillary column of RTX-5MS. The column temperature was initiated at 50℃, held for 5 min, increased at the rate of 3 ℃/min to 120 ℃, held for 2 min, and then increased at the rate of 4 ℃/min to 220℃, held for 10 min. Helium carrier gas was used at a constant flow rate of 1.3 mL/min. Mass conditions were ionization voltage, 70 eV; injector temperature, 250℃; ion source temperature, 250 ℃; splitting ratio, 30：1; full scan mode in the 40-500 Da mass ranges with rate of 0.2 s per scan. Attribution of the major characteristic peaks was identified for SHXW by comparing the chemical standards, references of Chinese herbal medicines and the negative controls of prescription samples （NC） of SHXW. With the help of the temperature-programmed retention indices （PTRIs） used together with mass spectra and chemical standards, 25 major characteristic peaks have been identified. Nine volatile medicinal materials were identified in the prescription of SHXW by attributing to the 27 major characteristic peaks. The results demonstrate that the proposed method is a powerful approach to quality control of complex herbal medicines.

Low polar volatile constituents from Isodon excisa by GC-MS

An attempt had been made to isolate and identify the low polar volatile constituents from Isodon excisa. The dried plants were heat extracted with ethanol and then extracted with petroleum ether. The constituents were isolated and analyzed by GC-MS and then we retrieved them on NIST08 mass spectrometry database to determine their structures. Finally, successful results were achieved, 111 compounds were obtained and identified. 105 of them were reported for the first time in lsodon excisa and 22 of them were first found in natural products. Thus, the main constituents of it were found to be Sitosterol （33.28%）, 3-Amino-4-pyrazolecarbonitrile （9.55%）

Anti-inflammation Activities of Essential Oil and Anti-microbial Activities Of Ethanol Extraction from China's Rosemary

Rosemary(Rosmarius officinalis L.), an endemic plant species in south region of China, is traditionally used as a spice. In this research, the anti-inflammatory activities of essential oil and the antibacterial activities of ethanol extraction were determined, respectively. Results showed that based on the GC-MS analysis there were 35 kinds of active ingredients in the essential oil in totally, mainly including D-limonene(24.158 ml/L), α-Pinene(23.325 ml/L), Camphor(9.855 ml/L),Camphene(7.076 ml/L), Verbenone(6.685 ml/L), Borneol(5.580 ml/L), etc. The LCUV determination indicated that the main components in the ethanol extractionwere rosmarinic acid(3 910 mg/kg) and carnosic acid(2 970 mg/kg). By mice peritoneal macrophage phagocytosis of chicken erythrocytes experiment, the essential oil of rosemary was shown having a significant role in anti-inflammation. And the ethanol extraction had broad-spectrum antibacterial effects, but had no effect on mold by the agar diffusion method of 8 bacteria. As a result, both rosemary essential oil and ethanol extraction had good potential medicinal values.

Study on the Antioxidant Component of Fermented Rice Bran by Bacillus Natto

Each component of rice bran fermentation(RBF)of Bacillus natto was extracted and its antioxidant activity was tested.By dint of thin layer chromatography,the antioxidant components were separated.The sample isolated from TLC for ethyl acetate phase and ether phase was analyzed by GC-MS.Results indicated that the antioxidant activity of large components in rice bran fermentation was low.The constituents of extracted phase had antioxidant activity apart from the petroleum ether phase.The constituents of ethyl acetate phase and Ether phase had best antioxidant activity,163 and 168 kU/g,respectively.The main composition of ethyl acetate phase was allyl group methyl-thioether and the main composition of ether phase included 3,5-dimethyl phenol,2,4-dipl-tert-Butyl and Fluazifop.