联用SPME与GC-MS技术分析新鲜、萎蔫、干枯枫杨挥发性成分

运用SPME与GC/MS联用技术从新鲜枫杨叶挥发性物质中共检测出化合物52种,主要成分是橙花叔醇(15.54%)、吉马烯A(14.22%)、反式子丁香烯(10.19%)、7,8,9,10-四氢化-S-三氮唑(3,4-A)-呔嗪(8.59%)、十六酸(6.22%);萎蔫枫杨叶挥发性物质中共检测出化合物32种,主要成分是α-红没药烯(17.69%)、橙花叔醇(16.64%)、反式子丁香烯(14.26%)、α-桉叶烯(9.14%);干枯枫杨叶挥发性物质中共检测出化合物31种,主要成分是反式子丁香烯(23.30%)、α-红没药烯(17.75%)、α-桉叶烯(12.69%)、橙花叔醇(8.35%)、杜松烯(7.O%).随着枫杨萎蔫程度的变化,三者含有的化合物组分以及其相对含量都发生变化.本研究是首次报道枫杨的挥发性化学成分分析.     

Composition of the essential oil from the lemon balm growing in the neighborhood of Krasnoyarsk as indicated by gas chromatography–mass spectrometry data

Essential oil has been isolated from the above-ground part of the lemon balm growing in the neighborhood of Krasnoyarsk by the method of exhaustive water and steam distillation. Forty seven components, each with a content of more than 0.1% of whole oil, have been identified by GC-MS. The main oil components are citronellol (36.71%) and geraniol (27.20%). The oil also contains ten components with a content of more than 1% of the sum of all oil components: benzyl alcohol (1.67%), linalool (1.75%), citronellal (1.44%), neral (3.33%), geranial (4.39%), caryophyllene (3.73%), caryophyllene oxide (1.40%), dibutyl phthalate (1.36%), butylisobutyl ester of phthalic acid (2.45%), and phytol (2.55%). The composition of lemon balm oils from different regions of the world has been compared.     

我国特有植物一木里香橼叶精油化学成分的研究

用气相色谱保留指数定性法、色谱-质谱-计算机联用测定和标准品迭加法分析了木里香橼叶精油的化学成分。从分离出的59个色谱峰中鉴定了31个化合物。其中主要成分是柠檬烯(31.730％)、芳樟醇(1.554％)、香茅醛(23.383％)、香茅醇(1.189％)、橙花醇(11.777％)、香叶醛(16.544％),乙酸香茅酯(1.427％)、乙酸橙花酯(2.258％)、乙酸香叶酯(4.714％)等。把木里香橼叶油与木里香橼果皮油与云南野香橼叶油分别作了比较。结果表明木里香橼叶油中含氧化合物醇、醛、酯的含量相当高,是精油的主要成分,可能作为进口橙叶油的较好的代用品,是一种很有潜力的天然香料资源。     

夜合花叶的精油成份研究

利用气相色谱—质谱—计算机联用技术对夜合花[Magnolia coco(Lour.)DC.]叶的精油成份进行了分析。从分离出的139个色谱峰中鉴定出25个化合物,其含量占总组成的66.358％,主要成份是β-松油烯(37.570％),松油醇4(6.504％),α-蒎烯(3.499％),去氢白菖蒲烯(2.758％),芳樟醇(2.440％),1-(1,5-二甲基-4-己烯)苯(2.436％)等。     

棘托竹荪挥发油化学成分及抑菌作用的研究*

利用水蒸汽蒸馏法提取棘托竹荪的挥发油,得油率为0.45%。.应用气相色谱—质谱联用系统首次对其挥发油的化学成分进行研究。以FFAP柱分离出36个峰,用质谱法鉴定出28个成分,其主要成分为13-甲基-环氧十四烷-2-酮 (23.53%)、亚油酸(17.56%)、芹子烯(12.37%)、棕榈酸(8.20%)、9-十六碳烯酸(7.84%)、(-)-Lepidozenal(7.82%)等, 占总挥发油的97.76%。对挥发油进行抑菌试验,其结果为:桔黄青霉、啤酒酵母最敏感, 黑根霉、黑曲霉次之,白色假丝酵母、金色葡萄球菌,大肠杆菌稍差。     

福建产小鱼仙草挥发油的含量及其化学成分的研究

应用气相色谱－质谱－计算机联用系统对小鱼仙草（Mosla dianthera Maxim),挥发油的化学成分进行研究,以SE－54石英毛细管柱分离出43个峰,用GC／MS鉴定出39个成分,其主要成分为百里香酚（37．15％）,香荆芥酚（14．85％）,丁香烯（5．75％）,芳樟醇（5．40％）,檀香烯（4．12％）,律草烯（3．61％）,香桧醇（2．87％）等,占总挥发油的98．40％,又应用气相色谱归一化法计算了各化学成分含量。     

Studies on the Chemical Constituents of Fruits of Lindera glauca (Sieb. et Zuec.) Bl. and Their Uses

The paper presents the chemical constituents of fruits of Lindera glauca (Sieb. et Zucc.) B1. By applying the techniques of fractional distillation, column chromatography, GC, TLC, PC, chemical methods and spectroscopic data (IR, NMR and MS), the following chemical constituents in essential oils from the fruits and the fatty acids of fatty oil from seed have been identified: There are 13 components in essential oil—α-pinene (0.03%), β-pinene (2.75%), camphene (2.27%), ocimene (77.99%), nonyl aldehyde (1.08%), capric aldehyde (0.30%), 1,8-cincol (2.47%), borneol (0.21%), citral (0.42%), β-cymene (0.63%), safrole (2.60%), bornyl acetate (0.60%), γ-patehoulene (0.69%); 6 fatty acids in fatty oilcaprylic acid (0.28%), eapric acid (55.27%), lauric acid (32.21%), myristic acid (1.18%), palmitie acid (2.72%) and stearie acid (8.94%). In addtion, the use of essential oil of fruit and fatty oil of seed has been studied.     

Ticks infesting domestic animals in Italy: current acarological studies carried out in Sardinia and Basilicata regions

The note reviews published and unpublished data on acaralogical studies carried out by different parasitologists' groups in Sardinia and Basilicata regions. In Sardinia 72 collecting sites were investigated and a total of 4,086 ticks were collected from hosts (cattle, sheep, goats and pigs) and from soil. So far 2,413 ticks belonging to six genera have been identified: Rhipicephalus (67.2%), Haemaphysalis (24.1%), Hyalomma (2.7%), Boophilus (0.7%), Dermacentor (4.9%), Ixodes (0.3%). Host-associated ticks were collected from 50 out of 200 selected farms in Basilicata. About 4,000 tick specimens were collected and 1,794 ticks have been identified (of which 1,215 were adults, 6 larvae and 573 nymphs). The following genera were identified: Ixodes (20%), Rhipicephalus (27%), Hyalomma (31%), Haemaphysalis (18%), Dermacentor (6%). The seasonal distribution of the species identified in the two regions studies is discussed from a geographical and climatic point of view.     

A Study on the Chemical Components of the Essentialoi from Peel of Citrus medica L. var. muhensis W. D. et Y.

The chemical components of the essential oil from peel of Citrus medica L. var. muliensis W. D. et Y. has been studied by means of the GC-MS-DS, the retention index of eapillarly gas chromatography and the Authentic sample addition process. Twenty-nine constituents has been identified from sixty-four seperated peaks. The main constituents is d-limonene (68.2%), geranial (9.5%), neral (5.37%), nerol (2.72%), β-ocimen (2.47%) and (+)-Carvone.     

Two unusual glycerophospholipids from a filamentous fungus, Absidia corymbifera

The chloroform-methanol extractable lipids of the soil filamentous fungus Absidia corymbifera VKMF-965 account for about 20% by weight of dry cells and are composed of low-polarity constituents (about 75% of the total lipids), such as triacylglycerols (mainly), diacylglycerols, sterols and free fatty acids, as well as of glycolipids (about 3%) and phospholipids. The last consist largely of components common to the fungal lipids, namely, phosphatidylethanolamine (38% of the total phospholipids), phosphatidyl-myo-inositol (16%), diphosphatidylglycerol (12%), phosphatidylcholine (7%), phosphatidic acid (6%) and phosphatidylglycerol (3%), and two unusual phospholipids, PL1 (6%) and PL2 (9%). Based on the infrared (IR), (1)H-nuclear magnetic resonance (NMR), (13)C-NMR and mass spectra along with the results of degradation experiment, these two phospholipids have been established to be 1,2-diacyl-sn-glycero-3-phospho(N-acetylethanolamine), or N-acetyl phosphatidylethanolamine, and 1,2-diacyl-sn-glycero-3-phospho(N-ethoxycarbonyl-ethanolamine), respectively. These structures have been confirmed by preparing similar phospholipids from the phosphatidylethanolamine isolated from the same fungus and correlating their chromatographic behaviour, IR and (1)H-NMR spectra with those of PL1 and PL2. So far N-acetyl phosphatidylethanolamine has been detected only in cattle and human brains and a human placenta but its structure was not rigorously proved. PL2 is a novel lipid; to our knowledge no natural phospholipid with an urethane group has yet been found. The main fatty acids of both the phospholipids are n-hexadecanoic, octadecanoic and octadecadienoic ones; PL2 contains in addition a considerable amount of octadecatrienoic acid with its greater portion located at the sn-1 position.     

Hereditary deafness in Kirov oblast: estimation of the incidence rate and DNA diagnosis in children

Genetic analysis of hereditary deafness (HD) has been performed in the city of Kirov and ten rural districts of Kirov oblast (administrative region). The analysis employed the methods used in audiology, medical genetic counseling, and DNA diagnosis. Deafness has been established to be hereditary in 143 children from 100 unrelated families. The incidence rates of isolated and syndromic HDs in the period studied (1995-2001) have been estimated at 1.25 and 0.36 per 1000 newborns, respectively, the total incidence rate of all HD forms being 1.61 per 1000 newborns (1 case per 621 newborns). DNA analysis for the detection of seven frequent mutations in the genes GJB2 (the 35delG, 167delT, 235delC, and M34T mutations), GJB6 (the del(GJB6-D13S1854) and del(GJB6-D13S1830) mutations), and TMC1 (the R34X mutation) has been performed in families with isolated neurosensory deafness. Molecular genetic analysis has detected mutations in 51 children (48.6%); in 54 children (51.4%), no mutations have been found. The following genotypes have been identified in children with HD: 35delG/35delG in 32 probands (30.5%), 35delG/+ in 16 probands (15.2%), 35delG/235delC in 1 proband (0.95%), M34T/+ in 1 proband (0.95%), and M34T/35delG in 1 proband (0.95%). The 167delT mutation has not been found. The frequency of the 35delG mutation in the GJB2 gene has been estimated to be 39.05%. In the group with a family history of HD, mutations have been found in 66.7% of patients; in the group without a family history of HD, in 37.5% of patients. No mutation has been found in the GJB6 or TMC1 gene. Molecular genetic analysis has been performed in a family with clinically diagnosed Treacher Collins-Franceschetti syndrome. Sequencing has been used to find the 748-69C>T polymorphism in intron 6 (in the homozygous state) and the 3635C>G mutation in exon 23 leading to the substitution of glycine for alanine at position 1176 of the amino acid sequence (Ala1176Gly, in the heterozygous state), which have not been described before.     

The HIV/AIDS epidemic and the trends in the behavior of people using injection narcotics (IDU)

The degree of risk of the spread of HIV infection among drug addicts in Zhitomir has been prognosticated. As revealed in this study, narcotic drugs are mostly introduced by individual dispensable syringes or by individual reusable syringes. But such factors as the repeated use of needles (47%), obtaining drug solution from different persons (49%), the injection of drugs under unsanitary conditions (62%), with-drawing drug solution into the syringe by some other person (32%), unavailability of the means of disinfection (64%), absence of knowledge and practice in disinfection (91%), the presence HIV-infected persons among IDU (41%), a low level of sanitary and hygienic culture (41%), lack of sexual restraint (93%), concubinage with IDU (44%), unemployment (66%), etc. have been found to increase the possibility of getting HIV infection twofold. The results of this sociological study have demonstrated new trends in the study of the behavior of IDU, necessary for the creation of the module for preventive work both in Zhitomir and the Zhitomir region.     

Hereditary deafness in Kirov oblast: Estimation of the incidence rate and DNA diagnosis in children

Genetic analysis of hereditary deafness (HD) has been performed in the city of Kirov and ten rural districts of Kirov oblast (administrative region). The analysis employed the methods used in audiology, medical genetic counseling, and DNA diagnosis. Deafness has been established to be hereditary in 143 children from 100 unrelated families. The incidence rates of isolated and syndromic HDs in the period studied (1995–2001) have been estimated at 1.25 and 0.36 per 1000 newborns, respectively, the total incidence rate of all HD forms being 1.61 per 1000 newborns (1 case per 621 newborns). DNA analysis for the detection of seven frequent mutations in the genes GJB2 (the 35delG, 167delT, 235delC, and M34T mutations), GJB6 (the del(GJB6-D13S1854) and del(GJB6-D13S1830) mutations), and TMC1 (the R34X mutation) has been performed in families with isolated neurosensory deafness. Molecular genetic analysis has detected mutations in 51 children (48.6%); in 54 children (51.4%), no mutations have been found. The following genotypes have been identified in children with HD: 35delG/35delG in 32 probands (30.5%), 35delG/+ in 16 probands (15.2%), 35delG/235delC in 1 proband (0.95%), M34T/+ in 1 proband (0.95%), and M34T/35delG in 1 proband (0.95%). The 167delT mutation has not been found. The frequency of the 35delG mutation in the GJB2 gene has been estimated to be 39.05%. In the group with a family history of HD, mutations have been found in 66.7% of patients; in the group without a family history of HD, in 37.5% of patients. No mutation has been found in the GJB6 or TMC1 gene. Molecular genetic analysis has been performed in a family with clinically diagnosed Treacher Collins-Franceschetti syndrome. Sequencing has been used to find the 748–69C>T polymorphism in intron 6 (in the homozygous state) and the 3635C>G mutation in exon 23 leading to the substitution of glycine for alanine at position 1176 of the amino acid sequence (Ala1176Gly, in the heterozygous state), which have not been described before.     

Occurrence of positional isomers of octadecenoic and hexadecenoic acids in human depot fat

Positional isomers of hexadecenoic aud octadecenoic acids of human adipose tissue have been separated by gas-liquid chromatography and their amounts determined by oxidative cleavage (MnO(4) and IO(4)). The following isomeric octadecenoic acids were present: 7-octadecenoic acid (0.4%), 8- (1.9%), 9- (73.0%), 10- (2.5%), 11- (19.0%) and 12- (3.2%). The hexadecenoic acids have also been shown to be a mixture of positional isomers, in which the cis-9-isomer predominates. 10-Hexadecenoic and 12-octadecenoic acids could conceivably be precursors of linoleic acid. The following branched fatty acids have also been determined in human depot fat: 13-methyltetradecanoic, 12-methyltetradecanoic, 14-methylpentadecanoic, 14-methylhexadecanoic, and 16-methylheptadecanoic acid. They were present in percentages of 0.02-0.6% and their identification rests solely on comparison of their gas-liquid chromatographic retention times with those of synthetic compounds.     

Comparative analysis of volatiles from needles of five-needle pines of northern and eastern Eurasia

The chemical composition of essential oil samples from needles of six species of five-needle pines (Pinus pumila, Pinus sibirica, Pinus parviflora, Pinus armandii, Pinus koraiensis, and Pinus cembra) and one natural interspecific hybrid Pinus sibirica × Pinus pumila has been studied by the chromato-mass spectrometry method. Essential oils have been prepared by simultaneous steam distillation-extraction. The analysis of the samples?? composition showed that the main constituents of the essential oils were the following mono- and sesquiterpenic compounds: ??-pinene (5?C63%), camphene (0.7?C3.6%), ??-pinene (0.7?C7%), ??-myrcene (0.5?C3.4%), 3-carene (0?C16%), limonene (0.6?C7.9%), ??-phellandrene (0.7?C5.3%), terpinolene (0.4?C6.7%), bornyl acetate (0.2?C12%), ??-terpenyl acetate (0?C4.6%), caryophyllene (0.4?C24%), humulene (0.1?C4%), germacrene D (0.1?C24%), bicyclogermacrene (0.1?C3.6%), ??-cadinene (0.9?C2.3%), ??-cadinene (2.2?C6.1%), germacrene D-4-ol (0?C6.8%), T-cadinol (0.7?C2.9%), and ??-cadinol (0.7?C6.0%).     

Virtual screening and in vitro assay of potential drug like inhibitors from spices against glutathione-S-transferase of filarial nematodes

Glutathione-S-transferase(s) (GST) enzyme from Brugia malayi has been exploited as a target in lymphatic filariasis therapeutics. An active GST is a homodimer of a 208 residue long monomer consisting of two domains, a smaller α/β domain and a larger α domain. The components of the glutathione (GSH) system, mainly GST enzymes, are critical antioxidant and detoxification system responsible for the long-term existence of filarial worms in mammalian host; hence they are major chemotherapeutic targets in filarial species. In the present study, 58 phytochemicals from 10 plants, predicted and reported to have potential nematicidal activity and ADMET satisfaction, have been docked to GST enzyme of B. malayi to assess their binding affinity and consequently their inhibitory activity. A comparative study has been made with commonly employed chemotherapeutic GST inhibitors such as cibacron-blue, butylated hydroxyanisole, hexyl glutathione and ethacrynic acid. In vitro effects of potential drug like compound from in silico results have been done for validation of docking studies. In vitro assay revealed efficacy in GST inhibition in the following compounds: linalool (97.50%), alpha-pinene (90.00%), strychnine (87.49%), vanillin (84.99%), piperine (79.99%), isoeugenol (62.49%), curcumin (57.49%), beta-caryophyllene (39.50%), cinnamic acid (27.49%), capsaicin (19.99%), citronellol (19.99%) and geraniol (17.49%). An online database () has been developed, which will serve as a useful repository of information on GST inhibitors for future development of drugs against filarial nematodes. These findings thus suggest that the above phytochemicals could be potentially developed as lead molecules for targeting GST of lymphatic filarial parasites.     

A Study on the Chemical constituents of the Volatile Oils from the Fresh Leaves of Camellia sinensis Kuntze

The fresh leaves of Camellia sienesis (L.) Kuntze were distilled under low temperature and reduced pressure, the distillate thereof was extracted with ether, which gave rise to the volatile oil. From the volatile oil, by applying the GC, TLC, and IR, 51 components have been analyzed and identified. In addition, the variation law of the aroma of the fresh tea leaves in spring, summer and autumn has also been studied and determined. The main aroma of the fresh leaves of Camellia sienesis (L.) Kuntze are: cis-3- hexen-l-ol (spring, 2.15%; summer, 3.13%; autumn, 15%), benzyl alcohol (spring, 1.23%; summer, 1.60%; autumn, 1.01%), trans-linalooloxide (furanoid) (spring, 4.23%; summer, 4.11%; autumn, 3.18%), linalool (spring, 19.84%; summer, 8.20%; autumn, 11.91%), trans-linalooloxide (pyranoid) (spring, 1.73%; summer, 1.28%; autumn, 0.91%), geraniol (spring, 25.46%; summer, 3.93%; autumn, 3.16%), trans-2-hexenal (spring, 3.52%; summer, 25.48%; autumn, 1.13%), β-ionone (spring, 0.31%; autumn, 0.02%), cis-jasmone (spring, 0.20%; summer, 0.17%; autumn, 0.05%).     

广西灵香草挥发油化学成分

灵香草(Lysimachia foenum-graecum Hance)又名零陵香,为报春花科(Primulaceae)排草属(Lysimachia L.)植物,主产广西、云南、广东、四川、贵州等地[1].灵香草性味甘、淡、平,具行气、止痛、驱蛔功能,药理实验证明具有抑制流感病毒作用[2]; 其挥发油香气浓郁且持久,是烟用香精的重要赋香剂之一.     

Nucleic acids and alkylating agents: carbon-13 magnetic resonance studies of the methylation of ribonucleic acid with methyl methanesulfonate.

Direct examination of the interaction of ribonucleic acid with the alkylating agent, methyl methanesulfonate, by carbon-13 magnetic resonance spectroscopy has demonstrated the potential usefulness of this new spectroscopic method in studying the interaction between nucleic acids and biologically active agents. By comparison with the model compounds isolated from the reactions of mononucleotides with methyl methanesulfonate, five methylated products, 7-methylguanosine (49.7%), 1-methyladenosine (21.2%), 3-methyl cytosine (12.7%), 1-methylguanosine (7.5%), and methyl phosphate (8.9%, tentative) have been identified in the alkylated RNA from the reaction without buffer, whose pH is maintained using a pH stat; three methylated products, 7-methylguanosine (61.1%), 1-methyladenosine (20.5%), and 3-methylcytosine (18.4%) have been identified from the reaction in phosphate buffer. These quantitative differences may account for the failure of previous structure-activity correlations. The limits of the biological interpretation of the present and previous chemical results are discussed.     

Identification and synthesis of a trisaccharide produced from lactose by transgalactosylation

Enzymatic transgalactosylation of lactose by means of Streptococcus thermophilus, subspecies DN-001065, led to a mixture of D-galactose (approximately 4%), D-glucose (approximately 15%), lactose (approximately 51%), minor disaccharides (6%), trisaccharides (approximately 20%) and tetrasaccharides (3%). The major trisaccharide (approximately 16%) was identified by NMR spectroscopy and chemical synthesis as being the known beta-D-galactopyranosyl-(1-->3)-beta-D-galactopyranosyl-(1-->4)-D-glucos e (3'-beta-D-galactopyranosyl-lactose). It was purified from a mixture of peracetylated oligosaccharides by column chromatography followed by deacetylation. For the first time, 3'-beta-D-galactopyranosyl-lactose has been obtained on the 1 g scale, by resorting to simple techniques and equipment. NMR spectra have been unambiguously assigned.