中国车前草挥发性化学成分分析

用同时蒸馏 萃取装置(SDE)提取中国车前草的挥发性物质,测得车前草挥发油质量分数为2.79%,用GC MS法从车前草的挥发油中分离确认出20种化学成分,占挥发油总量的95.08%。用峰面积归一化法通过化学工作站数据处理系统得出各化学成分在挥发油中的质量分数。     

侧柏叶的挥发性成分分析

侧柏叶(Platycladus orientalis(L.) Endl.)柏科(Cupressaceae)乔木侧柏的嫩枝及叶,侧柏叶别名扁柏、香柏、片柏、片松.全国各省区都有栽培,为我国特产[1].侧柏叶气清香,味苦涩、微辛[1].     

冠心苏合丸中挥发性成分的提取分析及其质量监控

采用了水蒸气蒸馏 萃取法和同时水蒸气蒸馏 萃取法提取冠心苏合丸中的挥发性组分,测得用两种方法提取的冠心苏合丸中的挥发性组分提取率分别为11%和14%。利用GC MS方法对两种方法所得的挥发性组分进行分析,通过G1701BA化学工作站检索NIST98谱图库,并结合标准谱图库和有关文献,从冠心苏合丸中的挥发性组分中分别确定出19种、14种化学成分,分别占冠心苏合丸中挥发性组分总检出量的95.89%和97.27%。用峰面积归一化法通过化学工作站数据处理系统,得出各化学成分在挥发性组分中的质量分数。主要挥发性组分是冰片、异冰片和苯甲酸苄酯。从两种方法提取的挥发性组分中确认的化学成分是否涵盖五味中药材具有代表性成分,可以很方便地进行质量监控和真伪鉴别。并采用气相色谱法对冠心苏合丸中冰片的含量进行了测定,作为辅助鉴别。结果,冰片浓度在1.0～5.0mg mL范围内与冰片对内标物的色谱峰面积比值成良好的线性关系,冰片的平均回收率为98%～106%。     

柠檬果茶中游离态和键合态挥发性成分分析

以柠檬果茶为研究对象,建立了顶空固相微萃取前处理结合气相色谱质谱联用技术测定其中挥发性化合物的分析方法。采用开水冲泡对样品进行提取,通过Amberlite XAD-2大孔吸附树脂对柠檬果茶中的糖苷类挥发性组分键合,分离游离态和键合态化合物,甲醇溶剂作为洗脱剂对键合态化合物进行洗脱,Almondsβ-D-葡萄糖苷酶对其酶解。使用气质联用对样品中游离态和键合态挥发性成分进行检测,其结果根据数据库匹配和对比文献保留时间定性,内标法进行定量。结果表明,柠檬果茶中含有游离态物质24种,键合态物质16种,主要为(+)-柠檬烯、1-辛醇、橙花醇、(-)-4-萜品醇、alpha-松油醇等。方法为花果茶干燥工艺提供参考。     

小叶香樟新鲜树叶挥发性成分分析

采用水蒸汽蒸馏和乙醚萃取收集小叶香樟新鲜树叶挥发油,经气质联用分析鉴定出49个化合物,占峰面积的95.9%,挥发油得率为1.73%。主要化合物的类型为单萜(86.4%)、倍半萜(10.0%)、芳香族(1.41%)和脂肪族(1.13%)。其中质量分数最高的为L-芳樟醇(45.9%),其次为樟脑(28.5%)和橙花叔醇(4.66%)。     

超临界流体萃取-GC-MS分析西黄丸中挥发性成分

建立西黄丸中挥发油成分乙酸辛酯的含量测定方法,为西黄丸的质控标准提供依据。方法:超临界CO2萃取西黄丸中挥发油成分,采用气相色谱法测定乙酸辛酯含量;研究压力、温度、时间和粒度因素对挥发油得率与乙酸辛酯含量的影响,并进行了化学计量学分析。采用GC-MS分析了适宜条件的挥发油的成分。综合考虑挥发油得率和乙酸辛酯含量双指标,确定的西黄丸挥发油萃取条件为:粉碎粒度为80目,萃取压力为25 MPa,温度为40℃,时间为2 h。在此条件下,挥发油得率达到7.76%,乙酸辛酯含量达到0.72 mg·g^-1。通过指纹图谱、主成分分析(PCA)、正交偏最小二乘判别分析(OPLS-DA)化学计量学分析可知,不同萃取条件对所提取的挥发油物质组分及其含量没有显著性差异。GC-MS鉴定出的主要成分有(1S-endo)-2-甲基-3-亚甲基-2-(4-甲基-3--3-戊烯基)-二环[2.2.1庚烷、10α-羟基日本刺参萜、(±)-麝香酮、4-亚甲基-2,8,8-三甲基-2-乙烯基-双环[5.2.0]壬烷和2-甲基-4-(2,6,6-三甲基-1-环己烯-1-基)丁醛。结论:西黄丸挥发油成分适宜萃取条件,及建立的乙酸辛酯含量测定方法准确、可靠,为有效控制西黄丸质量,完善其质量标准及进一步的药效成分研究提供了科学依据。     

Miniature radio-frequency mobility analyzer as a gas chromatographic detector for oxygen-containing volatile organic compounds, pheromones and other insect attractants

A high electric field, radio-frequency ion mobility spectrometry (RF-IMS) analyzer was used as a small detector in gas chromatographic separations of mixtures of volatile organic compounds including alcohols, aldehydes, esters, ethers, pheromones, and other chemical attractants for insects. The detector was equipped with a 2 mCi 63Ni ion source and the drift region for ion characterization was 5 mm wide, 15 mm long and 0.5 mm high. The rate of scanning for the compensation voltages was 60 V s(-1) and permitted four to six scans to be obtained across a capillary chromatographic elution profile for each component. The RF-IMS scans were characteristic of a compound and provided a second dimension of chemical identity to chromatographic retention adding specificity in instances of co-elution. Limits of detection were 1.6-55 x 10(-11) g with an average detection limit for all chemicals of 9.4 x 10(-11) g. Response to mass was linear from 2-50 x 10(-10) g with an average sensitivity of 4 pA ng(-1). Separations of pheromones and chemical attractants for insects illustrated the distinct patterns obtained from gas chromatography with RF-IMS scans in real time and suggest an analytical utility of the RF-IMS as a small, advanced detector for on-site gas chromatographs.     

顶空气相色谱质谱法分析避蚊贴中挥发性成分

采用顶空-气相色谱-质谱联用技术分析鉴定了4种避蚊贴中的挥发性物质.样品经90℃、45 min顶空后,采用GC-MS进行定性分析.用面积归一化法得出各组分的相对含量.结果表明:经NIST质谱数据库检索和文献对照,样品Ⅰ、Ⅱ、Ⅲ和Ⅳ分别检出并确定了33、39、39和24种成分.样品Ⅰ、Ⅱ、Ⅲ和Ⅳ主要成分分别为桉树醇(相对...     

Environment-sensitive fluorophores with benzothiadiazole and benzoselenadiazole structures as candidate components of a fluorescent polymeric thermometer

An environment-sensitive fluorophore can change its maximum emission wavelength (λ(em)), fluorescence quantum yield (Φ(f)), and fluorescence lifetime in response to the surrounding environment. We have developed two new intramolecular charge-transfer-type environment-sensitive fluorophores, DBThD-IA and DBSeD-IA, in which the oxygen atom of a well-established 2,1,3-benzoxadiazole environment-sensitive fluorophore, DBD-IA, has been replaced by a sulfur and selenium atom, respectively. DBThD-IA is highly fluorescent in n-hexane (Φ(f) =0.81, λ(em) =537?nm) with excitation at 449?nm, but is almost nonfluorescent in water (Φ(f) =0.037, λ(em) =616?nm), similarly to DBD-IA (Φ(f) =0.91, λ(em) =520?nm in n-hexane; Φ(f) =0.027, λ(em) =616?nm in water). A similar variation in fluorescence properties was also observed for DBSeD-IA (Φ(f) =0.24, λ(em) =591?nm in n-hexane; Φ(f) =0.0046, λ(em) =672?nm in water). An intensive study of the solvent effects on the fluorescence properties of these fluorophores revealed that both the polarity of the environment and hydrogen bonding with solvent molecules accelerate the nonradiative relaxation of the excited fluorophores. Time-resolved optoacoustic and phosphorescence measurements clarified that both intersystem crossing and internal conversion are involved in the nonradiative relaxation processes of DBThD-IA and DBSeD-IA. In addition, DBThD-IA exhibits a 10-fold higher photostability in aqueous solution than the original fluorophore DBD-IA, which allowed us to create a new robust molecular nanogel thermometer for intracellular thermometry.     

香格里拉产小叶杜鹃花挥发性成分的GC-MS分析

研讨香格里拉县小叶杜鹃花的挥发油化学成分,为进一步合理开发利用其药用资源提供试验依据。利用水蒸汽同时蒸馏萃取法(SDE)提取小叶杜鹃花的挥发性化学成分,通过气相色谱-质谱联用技术(GC-MS)对各个色谱峰定性,并采用色谱峰面积归一法获得各个化合物的相对含量。从小叶杜鹃花挥发油中共分离鉴定了73个色谱峰,占挥发油总量的85.53%。小叶杜鹃花挥发油主要成分有α-蒎烯(14.00%)、正二十三烷(9.51%)、7-甲氧基-2,2-二甲基-3-色烯(6.26%)、正二十烷(6.11%)、苯乙醇(5.10%)、1-Heneicosyl formate(4.60%)等。     

核桃楸叶挥发油化学成分分析

采用水蒸气蒸馏法提取核桃楸叶中的挥发油,从核桃楸叶挥发油中分离了57种化合物,用气相色谱/质谱联用法鉴定了51种化合物,占被分离化合物的89.46%,其中烃类(33种,48.03%)、酮类(1种,0.55%)、醇类(5种,25.94%)、酯类(6种,8.43%)、酸类(1种,0.62%)、含氧杂环类(4种,2.62%)及甲酰类(1种,0.65%)等7大类化合物,有3类(27种,51.19%)为已知药用成分,这些数据为新药开发提供了科学信息.     

Analysis of volatile components of drugs and explosives by solid phase microextraction-ion mobility spectrometry

Current ion mobility spectrometry (IMS) devices are used to detect drugs and explosives in the form of particles and, in cases where the vapor pressure of the drugs or explosives is sufficiently high, the gas can be sampled and detected directly. The aim of this study is to demonstrate the use of solid phase microextraction (SPME) as a preconcentration technique coupled to an IMS for the detection of odor signature compounds of drugs and explosives. The reduced mobilities (K(o)) and IMS operating conditions for the odor signature compounds of cocaine, marijuana, and 3,4-methylenedioxy-N-methylamphetamine (MDMA) are reported for the first time. LODs, linear dynamic ranges (LDRs), and the precision of the analysis of these odor signature compounds, and the explosive taggant 2,3-dimethyl-2,3-dinitrobutane (DMNB) were obtained by SPME-IMS and normal IMS conditions. The systematic optimization of the IMS operating parameters for the detection of these odor compounds is also reported incorporating the use of genetic algorithms (GAs) for finding the optimal settings for the detection of these compounds of interest. These results support the case for targeting volatile components as a presumptive detection for the presence of the parent compounds of drugs and explosives. Furthermore, the IMS-specific GA developed can be used as an optimization tool for the detection of other compounds of interest in future work.     

GC-MS分析大叶金花草中挥发性成分和脂肪酸

应用 GC-MS 联用技术对大叶金花草(Stenoloma chusana(L.)Ching)的挥发性成分和脂肪酸进行了检测,共检测出7种挥发性成分和32种脂肪酸,脂肪酸检出量为87.65%,其中饱和脂肪酸占脂肪酸总量的53.13%,不饱和脂肪酸占脂肪酸总量的46.87%.该研究为大叶金花草的进一步开发利用提供了科学依据.     

Analysis by gas chromatography-mass spectrometry of the volatile components of Teucrium lusitanicum and Teucrium algarbiensis

The essential oils from four samples of Teucrium lusitanicum and one sample of Teucrium algarbiensis, grown in Algarve (southern Portugal) were analyzed by gas chromatography (GC) and gas chromatography-mass spectroscopy (GC-MS). Seventy-one volatile compounds were identified. Major compounds of T. algarbiensis oil were alpha-pinene (8.3%), sabinene (7.2%), beta-pinene (10.2%), limonene (11.8%) and germacrene D (7.6%). Concerning T. lusitanicum, some quantitative differences were found with regards to the major constituents of the oils from four populations: alpha-pinene (0.8-8.5%), sabinene (2.1-9.6%), beta-pinene (2.5-11.9%), limonene (1.2-11.5%) and elemol (2.6-12.0%).     

Determination of volatile components of systems not in thermodynamic equilibrium

A review is given of the literature on the analysis of complex mixtures of organic compounds and a procedure proposed for the separation and identification of the components of such mixtures. Retention data obtained with several chromatographic columns are combined with information from mass and Fourier-transform infrared spectra and identifications made with the aid of a computer.     

Sicilian lemon oil: Composition of volatile and oxygen heterocyclic fractions and enantiomeric distribution of volatile components

A total of 92 samples of Sicilian lemon oils (Citrus limon (L.) Burm. f.) produced from September 2008 to June 2009, industrially cold-pressed by different extraction techniques (Brown Oil Extractor and Food Machinery Corporation), were analyzed by GC-flame ionization detector (FID) and GC/MS-LRI to investigate the volatile fraction; by RP-HPLC/PDA to determine the non-volatile components and by enantio-GC-FID to determine the enantiomeric ratios of 12 volatile components. This study provides a detailed investigation on the composition of Sicilian lemon essential oils industrially produced during a productive season, with the aim to recognize quality parameters for the characterization of this product. The results obtained are discussed to evaluate seasonal variation, influence of the extraction techniques, and are compared with those obtained for samples produced during different seasons.     

固相微萃取/加速溶剂萃取-气相色谱-质谱法分析青山绿水茶叶的挥发性成分

采用固相微萃取(SPME)和加速溶剂萃取(ASE)两种前处理方法从青山绿水茶叶(也叫苦丁茶)中提取挥发性成分,用气相色谱-质谱法(GC-MS)定性。实验结果表明:两种前处理方法共检测出91种成分,SPME检出49种,ASE检出56种,共同组分14种。青山绿水茶叶的挥发性成分主要成分有β-月桂烯、3,3,5-三甲基-1,5-庚二烯、L-柠檬烯、α-罗勒烯、β-罗勒烯、β-蒎烯、2-甲基安息香醛和5-羟甲基糠醛等物质。这两种提取方法各具优势,共同应用可以起到取长补短的作用。     

固相微萃取结合气-质联用分析麻椒挥发性成分

以四川广元产的麻椒为原料,利用固相微萃取技术对麻椒中的挥发性成分进行提取,分别用装有HP-5ms和HP-INNOWAXms两种色谱柱的GC-MS进行分离与鉴定;采用质谱与保留指数进行定性,共鉴定出99种成分,其中烯烃类58种、醛类15种、醇类9种、酯类7种、酮类3种、其他烃类4种、其他化合物3种。采用面积归一化法确定了它们相对含量,含量较高的有芳樟醇、D-柠檬烯、β-崖柏烯、β-水芹烯、β-月桂烯、β-蒎烯、(-)-右旋吉玛烯、石竹烯、γ-萜品烯、3-崖柏烯、(Z)-β-罗勒烯、(1R)-(+)-α-蒎烯、(+)-3-蒈烯、(Z,Z,Z)-1,5,9,9四甲基-1,4,7环-十一碳三烯、萜品油烯。从鉴定出的挥发性成分的香气特征可知,烯烃类、醇类和醛类对麻椒的香气贡献较大。