GC-MS分析九头狮子草挥发油的化学成分

采用水蒸气蒸馏法提取九头狮子草挥发油,利用 GC-MS 联用技术,结合化学计量方法对其化学成分进行定性和定量分析,用面积归一法测定各组分的相对质量分数.结果表明：九头狮子草中挥发油主要由植酮(19．82％)、丁香油酚甲醚(3．96％)、β-石竹烯(3．75％)、肉豆蔻醚(3．08％)、3-甲基-2-(3,7,11-三甲基十二烷基)呋喃(3．64％)、2-戊基呋喃(2．73％)和氧化石竹烯(2．69％)等51种成分组成,占总量的98．82％.     

枯盘斑多毛孢Pf-毒素组分的研究Ⅰ．活性组分Ⅰ的结构分析

以正丁醇：水：甲醇(4：2：1)作洗脱剂,通过硅胶H60型柱反复柱层析,将3种有致病活性的物质充分纯化,在-40℃下冷冻干燥后,它们为褐色深浅不一的蓬松状物质,且极易吸潮。活性组分Ⅰ(Rf0．83)、活性组分Ⅱ(Rf0．79)和活性组分Ⅲ(Rf0．80)对马尾松切根幼苗和湿地松切根幼苗针叶都有致萎作用,通过质谱(MS)、核磁共振谱(^1HNMR、)和红外光谱(IR)等分析手段确定出所分离的活性组分Ⅰ的化学组成为C5H11O5N(M=165)。     

鞭檐犁头尖中的苯丙素甙类化合物

从天南星科植物鞭檐犁头尖的根茎中分离得到3个化合物,运用波谱技术(UV,IR,^1HNMR,^13C NMR and 2D NMR)对它们的化学结构进行解析,分别鉴定为松柏甙(1),甲基松柏甙(2)和硝酸钾(3)。从鞭檐犁头尖中分离得到苯丙素甙类化合物尚属首次。     

王不留行中刺桐碱的分离鉴定及抗炎活性研究

利用有机溶剂萃取、制备型薄层层析、半制备高效液相色谱三步分离法从王不留行中分离出生物碱物质,鉴定并探讨其抗炎活性。王不留行种子经石油醚脱脂、乙醇回流提取,二氯甲烷、乙酸乙酯、水饱和正丁醇依次萃取,获得水饱和正丁醇相(组分A3)。组分A3经制备型薄层层析分离,展开剂为正丁醇-乙酸乙酯-水(4∶1∶5,上层),于紫外灯254 nm、365 nm下检视,分为7个组分(组分B1~B7)。含量高且峰形简单的组分B2经半制备高效液相色谱分离,甲醇-水作为流动相,获得1个单体化合物(样品I)。经HPLC分析,样品I纯度高于98%。通过化学反应、UV、IR、LC-MS、1H NMR、13C NMR多种波谱分析方法对该化合物进行结构解析,确定其分子式为C14H18N2O2,化学名称为N,N,N-三甲基色氨酸,中文名为刺桐碱(hypaphorine),属于吲哚类生物碱。再采用二甲苯致小鼠耳廓肿胀的炎症模型,观察刺桐碱的抗炎效果。连续给药6 d后,刺桐碱剂量为25 mg·kg-1时,可显著抑制小鼠耳廓肿胀,肿胀抑制率为52.02%。与阿司匹林(200 mg·kg-1)的肿胀抑制率(67.48%)相比,无显著性差异。本研究首次采用一条新工艺路线获得王不留行刺桐碱,并发现其在整体水平上具有抗炎活性,有望成为化学一类新药的候选分子。     

王不留行中刺桐碱的分离鉴定及抗炎活性研究北大核心CSCD

利用有机溶剂萃取、制备型薄层层析、半制备高效液相色谱三步分离法从王不留行中分离出生物碱物质,鉴定并探讨其抗炎活性。王不留行种子经石油醚脱脂、乙醇回流提取,二氯甲烷、乙酸乙酯、水饱和正丁醇依次萃取,获得水饱和正丁醇相(组分A3)。组分A3经制备型薄层层析分离,展开剂为正丁醇-乙酸乙酯-水(4∶1∶5,上层),于紫外灯254 nm、365 nm下检视,分为7个组分(组分B1~B7)。含量高且峰形简单的组分B2经半制备高效液相色谱分离,甲醇-水作为流动相,获得1个单体化合物(样品I)。经HPLC分析,样品I纯度高于98%。通过化学反应、UV、IR、LC-MS、1H NMR、13C NMR多种波谱分析方法对该化合物进行结构解析,确定其分子式为C14H18N2O2,化学名称为N,N,N-三甲基色氨酸,中文名为刺桐碱(hypaphorine),属于吲哚类生物碱。再采用二甲苯致小鼠耳廓肿胀的炎症模型,观察刺桐碱的抗炎效果。连续给药6 d后,刺桐碱剂量为25 mg·kg-1时,可显著抑制小鼠耳廓肿胀,肿胀抑制率为52.02%。与阿司匹林(200 mg·kg-1)的肿胀抑制率(67.48%)相比,无显著性差异。本研究首次采用一条新工艺路线获得王不留行刺桐碱,并发现其在整体水平上具有抗炎活性,有望成为化学一类新药的候选分子。     

樱草杜鹃挥发油化学成分的研究

采用自制的水蒸汽蒸馏—溶剂萃取结合装置从樱草杜鹃提取出挥发油,用毛细管气相色谱-质谱法和Kovats指数双重定性法从樱草杜鹃挥发油中分离出65种成分,从其中鉴定出26个化合物,占总挥发油含量的91.91％。经冷冻分离和重结晶纯化所得的无色针状结晶,通过熔点测定,MS、IR、~1HNMR和UV分析,确定其结构为β-桉叶油醇。     

山石榴果实挥发油的化学成分分析

采用超临界CO2提取山石榴果实挥发油,并利用GC-MS联用技术分析挥发油的化学组成。从山石榴果实挥发油中分离、鉴定出33个化合物,占挥发油总量的89.43%。挥发油主要由各种酯、脂肪酸成分组成,含量较高的成分是11,14-二十碳二烯酸甲酯(11,14-eicosadienoic acid,methyl ester,42.49%),棕榈酸(pal mitic acid,15.34%),硬脂酸(stearic acid,10.54%),肉豆蔻酸(myristic acid,6.26%),十六酸乙酯(hexa-decanoic acid,ethyl ester,5.84%)。     

桂产罗勒挥发油化学成分的分析

采用GC-MS法建立桂产罗勒挥发油的化学成分分析方法。采用水蒸汽蒸馏法提取罗勒挥发油,用GC-MS联用技术分离并鉴定其成分,并用面积归一化法测定成分的相对含量。共鉴定出54个化合物,占挥发油总量的90.21%。桂产罗勒挥发油的主要成分是对烯丙基茴香醚、(+)表-双环倍半水芹烯、3,7,11-三甲基-(Z,E)-1,3,6,10-十二碳四烯,与文献报道的其他产地的罗勒油的化学成分存在显著差异。     

心草挥发油成分的研究

首次研究新疆产心草全草的挥发油成分 ,运用气相色谱 质谱 计算机联用技术 ,结合标准谱库 ,从检出的 87个化合物中共鉴定了 73种成分 ,其中主要成分为 1 丙氧基 2 丙醇、肉豆蔻醚、1,2 ,3 三甲氧基 5 (2 丙烯基 ) 苯、顺式 细辛脑、正己烷、芹菜脑、二甲醚、1,2 二甲氧基 4 (2 丙烯基 ) 苯、乙酸乙酯、斯巴醇、α ,α 4 三甲基 苯甲醇、反式 甲基异丁香油酚、水芹烯等 ,而 1 丙氧基 2 丙醇含量最高 ,占挥发油总量的 2 0 77% ,检出成分占挥发油总量的 92 4 6 %。     

稠李(Prunus padus Linn.)挥发油化学组成分析

采用GC-MS联机测定的分析方法,分析了稠李(臭李子)Prunus padus Linn.挥发油的化学组成,共分离出了三个组分,其主要成分为苯甲醛,占挥发油总含量的88.4%。     

β-环糊精包合红松籽油的制备工艺及生物利用度评价

介绍了单因素法优化红松籽油包合物的制备工艺,在最优条件下制备的红松籽油包合物固化率为70.95%,包合物含油率为26.88%。且对红松籽油和红松籽油包合物脂肪酸组分、粒径、电位和生物利用度进行对比。研究结果表明,包合物中红松籽油的各组分含量与红松籽油中各组分含量无明显差异,其中皮诺敛酸的含量为14%~16%。红松籽油包合物的平均粒径为177.3±2.6 nm,电位为-33.01±1.4 mV。红松籽油包合物组的血药最大浓度（Cmax）是红松籽油组的1.27倍,t1/2a是红松籽油的1.42倍;AUC值是红松籽油1.56倍;平均滞留时间（MRT）是红松籽油的1.04倍。因此,通过本实验说明红松籽油包合物与水溶液形成乳剂,粒径减小,水溶性增大,增加了包合物在体内的t1/2a和平均滞留时间（MRT）,提高了皮诺敛酸在体内的吸收。     

Metabolism of dibenzothiophene by a Beijerinckia species.

Beijerinckia B8/36 when grown with succinate in the presence of dibenzothiophene, accumulated (+)-cis-1,2-dihydroxy-1,2-dihydrodibenzothiophene and dibenzothiophene-5-oxide in the culture medium. Each metabolite was isolated in crystalline form and characterized by a variety of chemical techniques, cis-Naphthalene dihydrodiol dehydrogenase, isolated from Pseudomonas putida, oxidized (+)-cis-1,2-dihydroxy-1,2-dihydrodibenzothiophene to a compound that was tentatively identified as 1,2-dihydroxydibenzothiophene. The same product was formed when crude cell extracts of the parent strain of Beijerinckia oxidized (+)-cis-1,2-dihydroxy-1,2-dihydrodibenzothiophene under anaerobic conditions. Further metabolism of 1,2-dihydroxydibenzothiophene by heat-treated cell extracts led to the formation of 4[2-(3-hydroxy)-thionaphthenyl]-2-oxo-3-butenoic acid. The latter compound was metabolized by crude cell extracts to 3-hydroxy-2-formylthionaphthene. Further degradation of this metabolite was not observed.     

Metabolism of dibenzothiophene by a Beijerinckia species

Beijerinckia B8/36 when grown with succinate in the presence of dibenzothiophene, accumulated (+)-cis-1,2-dihydroxy-1,2-dihydrodibenzothiophene and dibenzothiophene-5-oxide in the culture medium. Each metabolite was isolated in crystalline form and characterized by a variety of chemical techniques, cis-Naphthalene dihydrodiol dehydrogenase, isolated from Pseudomonas putida, oxidized (+)-cis-1,2-dihydroxy-1,2-dihydrodibenzothiophene to a compound that was tentatively identified as 1,2-dihydroxydibenzothiophene. The same product was formed when crude cell extracts of the parent strain of Beijerinckia oxidized (+)-cis-1,2-dihydroxy-1,2-dihydrodibenzothiophene under anaerobic conditions. Further metabolism of 1,2-dihydroxydibenzothiophene by heat-treated cell extracts led to the formation of 4[2-(3-hydroxy)-thionaphthenyl]-2-oxo-3-butenoic acid. The latter compound was metabolized by crude cell extracts to 3-hydroxy-2-formylthionaphthene. Further degradation of this metabolite was not observed.     

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。     

Comparison of Three Different Extraction Methods on Osmanthus Volatile Oil: Aroma and Biological Activity

The osmanthus volatile oil was welcomed by consumers even if the high price since the unique and pleasant odor. Meanwhile, the low yield of osmanthus volatile oil restricts industrial production. In this work, an osmanthus volatile oil was obtained by means of a novel ultrasonic-assisted flash extraction method and was compared with the oil from hydrodistillation and supercritical fluid extraction on yield, aroma, and biological activities. The volatile oil obtained from the ultrasonic-assisted flash extraction was obtained with the petroleum ether and got a high yield at 3.51 % within a 40-min process, an increase of nearly 81 % from the single solvent extraction. This oil also showed a high aroma intensity and aroma compound concentration. Meanwhile, the oil also has the highest antioxidant ability but lower antibacterial activity against oil from hydrodistillation. It was considered that this work was helpful for the optimization of the extraction method of osmanthus volatile oil.     

北京萤火虫复眼的光学成像*

本文利用光学成像方法,研究了不同适应状态下的北京萤火虫phrococelia Pekininsis复眼所成的光学重叠像以及复眼的视场角。不同适应状态的晶体柱都能在距离复眼表面300-350μm之处形成光学重叠像。经过暗适应的晶体柱可以对不同物距的目标形成清晰的正重叠像,像的大小随物距的增大而减小;经明适应的晶体柱,成像物距范围变小,重叠像的像面亮度降低;经过漂白处理的晶体柱只能对一定的物距成像,像面亮度最低。 不同数目的晶体柱都能形成一重叠像,并随着其数目的增加,像面亮度也逐渐增强。根据对局部复眼视场范围的观察和其结构特征的了解,认为萤火虫单个复眼的视场角大于180度。     

Cytotoxic activity and constituents of the volatile oil from the roots of Patrinia scabra Bunge

The volatile oil from the roots of Patrinia scabra Bunge was isolated by steam distillation, and separated into four major fractions (Fr. A-D) by means of column chromatography. A total of 39 compounds (1-39) were identified by GC/MS analysis, and evaluated for their in vitro cytotoxic activities against human ovarian carcinoma cells (HO-8910) and human hepatoma cells (Bel-7402) (Table 1). Fr. A showed the strongest inhibitory effect on HO-8910 (IC50 = 21 microg/ml) and Bel-7402 cells (16 mcirog/ml), whereas Fr. B was the least active (>100 microg/ml). By comparison of the constituents of the four fractions, we assume that the cytotoxicity of the volatile oil of P. scabra is mainly due to the lignans and azulenes, rather than to caryophyllene oxide I (18). Our results suggest that the volatile oil of P. scabra possesses potent and tumor-specific cytotoxicity, and could serve as a possible candidate for future cancer chemotherapy.     

On the Chemical Study of the Volatile Oil ot Lysimachia Foenumgraecum Hance

The present paper reports that 0.17% fragrant, yellowish green colored volatile oil was obtained from Lysimachia foenumgraecum Hance by steam distil- lation with the following physical constants: nD20 1.4824, d1515 0.9059, [α]D25 -18.6 (c=1.1,CHCl3). 2. From the volatile oil a large amount of palmitic acid was separated and identified by its rap, elementary analysis and IR. 3. The volatile oil was divided into the acidic portion, the constituents in which were later transferred into their methyl esters (A), and the neutral and phenolic por- tion (B). (A) and (B) were analyzed by GC and GC-MS. The result of analysis showed that a total of 59 chemical constituents were indentified in the volatile oil; (A) con- sisted of 20 and (B) consisted of 39 constituents. 4. From the results as shown in the GC figures I and 2, hexahydrofarnesylacetone, being a rarely occured constituent in the natural product, and dibutyl phthalate might be considered to be the principal neutral costituents, just as the hexadecanoic acid and margaric acid to be the principal acidic constituents in the volatile oil of Lysimachia foenumgraecum Hance.     

The steam volatile oil of Wollemia nobilis and its comparison with other members of the Araucariaceae (Agathis and Araucaria)

The leaf essential oil of Wollemia nobilis (Wollemi Pine) has been investigated and compared with other members of the family Araucariaceae. All araucaroids examined yielded steam volatile oils in low yields. The oil from Wollemia nobilis was composed mainly of (+)-16-kaurene (60%), together with alpha-pinene (9%) and germacrene-D (8%). Oils from Agathis species endemic to Australia were high in monoterpenes, in contrast to those isolated from extra-Australian species. The major constituents of A. atropurpurea oil were phyllocladene (13%) and 16-kaurene (19%), followed by alpha-pinene (8%) and delta-cadinene (9%). A. microstachya yielded oil in which alpha-pinene (18%) was the major component; the only other components in excess of 5% were myrcene (7%), bicyclogermacrene (6%) and delta-cadinene (6%). A. robusta oil contained spathulenol (37%) and rimuene (6%). Approximately 40% of the oil was unidentified sesquiterpenes. A. australis oil contained 16-kaurene (37%), sclarene (5%) and an unidentified oxygenated diterpene K (12%) as major components; the only other compound in excess of 5% was germacrene-D (9%). 5,15-Rosadiene (60%), and 16-kaurene (7%) were the major constituents of A. macrophylla oil. A. moorei oil was rich in sesquiterpenes, but the only compounds in excess of 5% were allo-aromadendrene (6%), germacrene-D, delta-cadinene (10%), an unidentified sesquiterpene (12%) and 16-kaurene (6%). In A. ovata oil the most significant compounds were caryophyllene oxide (15%) and phyllocladene (39%). Araucaria angustifolia contained germacrene-D (9%) and the diterpenes hibaene (30%) and phyllocladene (20%) as major components of its essential oil. Oils of A. bidwillii, A. columnaris and A. cunninghamii were all low in mono- and sesquiterpenes and high in diterpenes. In the first, hibaene (76%) was the major constituent; the second contained hibaene (9%), sclarene (6%), luxuriadiene (13-epi-dolabradiene)(23%) and two unidentified diterpene hydrocarbons (B) (33%) and (E) (10%). In the last, 16-kaurene (53%) was the most significant component followed by hibaene (29%). A. heterophylla was unusual in that over half the oil was made up of the monoterpenoid alpha-pinene (52%), with phyllocladene (32%) being the only other compound of significance. alpha-Pinene (18%) was a significant component of A. hunsteinii oil; sclarene (11%) and germacrene-D (5%) were the only other compounds present in concentrations of more than 5%. A. luxurians oil was composed of 5,15-rosadiene (20%) and luxuriadiene (13-epi-dolabradiene) (66%), previously unreported from natural sources. The major components of A. montana were phyllocladene (61%) and 16-kaurene (23%). Sclarene (20%), luxuriadiene (19%) and the unidentified diterpene hydrocarbons (B) (25%) and (E) (10%) were the most important constituents of A. muelleri oil. A. scopulorum contained large amounts of 16-alpha-phyllocladanol (41%) as well as luxuridiene (10%) and delta-cadinene and alpha-copaene, both at 6%.     

胜红蓟化感物质之间相互作用的研究

 通过柱层析从胜红蓟挥发油中分离出早熟素Ⅰ、早熟素Ⅱ、子丁香烯、3,3-二甲基-5-特丁基茚酮、红没药烯、乙酸葑醇酯等6种主要化感物质(占挥发油总量的97％),并研究了这些化感物质在挥发、淋溶(饱和水溶液)和土壤降解途径下对萝卜,番茄和绿豆幼苗的化感作用。结果表明：早熟素Ⅰ、早熟素Ⅱ、3,3-二甲基-5-特丁基茚酮及子丁香烯(挥发途径)虽有较强的化感活性,但均弱于挥发油的化感活性,而子丁香烯(淋溶途径),红没药烯和乙酸葑醇酯则基本无化感活性。但是,早熟素n和无活性的三个化感物质结合,则表现出强烈的化感活性,说明胜红蓟各化感物质之间存在着明显的协同作用。