复方加味温胆汤挥发性成分分析

目的:研究复方加味温胆汤中的挥发性成分,探讨其治疗自闭症及相关症状的药效物质基础。方法:分别采用顶空固相微萃取法(HS-SPME)、水蒸气蒸馏法(SD)结合气质联用技术(GC-MS)对复方中挥发性成分进行分析鉴定;采用HS-SPME-GC-MS对煎煮前后复方挥发性成分进行对比分析。结果:共鉴定复方挥发性成分187种,含量最高的为α-细辛醚,D-柠檬烯次之。采用SD-GC-MS检测出74种,鉴定出66种,占挥发性成分总量99.89%;采用HS-SPME-GC-MS从煎煮前复方中检测出挥发性成分104种,鉴定出85种,占总挥发性成分的99.79%,从煎煮后复方中检测出挥发性成分77种,鉴定出65种,占总挥发性成分95.45%。结论:复方中α-细辛醚、D-柠檬烯和右旋龙脑等5种挥发性成分具有调节中枢神经系统、改善大脑功能、抗惊厥和安定等作用,能够改善自闭症的症状。本研究为复方加味温胆汤的挥发性成分分析提供了方法学基础,同时也为其治疗自闭症药效物质基础研究提供了参考依据。     

花蕾期延长型金银花挥发性成分研究

以传统金银花品种大毛花为对照,采用顶空固相微萃取气相色谱质谱联用技术,分析比较花蕾期延长型北花1号品种金银花的挥发性成分。采用面积归一化法测定其挥发性成分相对含量,共鉴定出52种挥发性成分,其中北花1号39种,大毛花33种,二者共有成分20种。北花1号在醇类、烃类含量上显著高于大毛花,而在酮类含量上显著低于大毛花,其中烟酸甲酯,棕榈酸甲酯,苯乙酮,己酸等20种化合物只在北花1号品种检测到。     

降香及其伪品挥发性成分对比研究

目的 分析降香及其伪品挥发性成分的异同点,为降香的真伪优劣鉴别提供科学依据,并为降香的进一步研究提供参考.方法 采用顶空固相微萃取法(HS-SPME)结合气质联用(GC-MS)技术对降香及其伪品挥发性成分进行分析鉴定,并用面积归一化法计算各成分的相对百分含量.结果 共检测出70种成分,鉴定出38种成分,主要为烯类、醇类和醛酮类,从降香挥发性成分中检测出42个峰,鉴定出25个成分,占挥发性成分的96.54%;从其伪品中检测出28个峰,鉴定出19种成分,占挥发性成分的80.7%.结论 降香及其伪品的挥发性成分差异较大,两者共有的成分有6种,含量差异大,降香的主要成分为橙花叔醇,占挥发性成分的61.47%,其伪品的主要成分为β-芹子烯,占总挥发性成分的59.04%.本实验为降香真伪优劣的鉴别提供科学指导,同时为降香的进一步开发提供参考依据.     

Volatile composition of Catharanthus roseus (L.) G. Don using solid-phase microextraction and gas chromatography/mass spectrometry

A total of 88 volatile and semi-volatile components were formally or tentatively identified in flowers, leaves and stems of Catharanthus roseus (L.) G. Don (cv. Little Bright Eye), by headspace solid-phase microextraction (HS-SPME) and by dichloromethane extraction, combined with gas chromatography–mass spectrometry (GC–MS). These include some diterpenic compounds (manool and manoyl oxides), a sesquiterpen (α-bisabolol), and some pyridine, pyrazine, indol and carotenoid derivatives. Applying multivariate analysis (principal component analysis and agglomerative hierarchic cluster analysis) to the HS-SPME–GC–MS data, it was possible to characterize each part of the vegetal material using a relative small number of compounds. Hence, flowers were richer in terpenic molecules (including limonene), α-bisabolol, methyljasmonate, cis-jasmone, 2-phenylethanol, phenylacetaldehyde, trans-2-octenal, benzylic alcohol and 2-isobutyl-3-methoxypyrazine. Leaves can be characterized by the methyl and propyl esters of fatty acids, mono- and disaturated, trans-phytol, carotenoid derivative compounds, hydrofarnesylacetone, methylanthranilate, manool and epi-manool oxide, while stems have high levels of volatile aldehydes, such as hexanal, octanal, cis-2-nonenal, cis-2-decenal, cis, trans-2,6-nonadienal, trans, trans-2,4-decadienal and cis, trans-2,4-decadienal. Dichloromethane extraction allowed also the identification of some alkaloid-like compounds that were not detected by HS-SPME.     

海南产高良姜叶和花挥发性成分分析

目的分析海南产高良姜叶和花挥发性成分分析并进行比较。方法采用顶空固相微萃取高良姜叶和花的挥发性成分,气相色谱-质谱联用技术检测其成分,峰面积归一化法计算各成分的相对质量分数。结果从高良姜叶中鉴定出32种成分,占色谱总流出峰面积的83.94%,主要是由萜类、酚(醇)类、酯类、酮类和烷烃类组成,其中4-氨基-1-萘酚(13.97%)、3-氯苯基-β-苯丙酸酯(10.33%)、石竹烯(9.85%)、苄丙酮(8.26%)、β-蒎烯(7.63%)和棕榈酸(3.44%)等化合物含量较高;从高良姜花中鉴定出16种成分,占色谱总流出峰面积的64.99%,主要由酚(醇)类、萜类和酸类组成,其中4-氨基-1-萘酚(20.61%)、石竹烯(10.93%)、棕榈酸(9.15%)、3-苯基-2-丁酮(5.92%)、苯丙醛(2.74%)、β-水芹烯(2.71%)和芳樟醇(2.28%)等化合物含量较高。结论良姜叶和花中的挥发性成分有很大的差异,本结果可为进一步开发利用该植物资源提供理论依据。     

顶空固相微萃取结合气质联用分析升麻蜜炙前后挥发性成分

目的：分析升麻及其炮制品挥发性成分的异同点。方法：采用顶空固相微萃取法（HS-SPME）结合气质联用技术（GC-MS）对升麻及其炮制品挥发性成分进行分析鉴定,用峰面积归一化法计算各成分的相对百分含量。结果：从升麻生品挥发性成分中分离出43个峰,鉴定出31个成分,占总挥发性成分的93.70%,含量最高的是y-柠檬烯,占总挥发性成分的36.28%;从其炮制品中分离出36个峰,鉴定出28种成分,占总挥发性成分的97.11%,含量最高的是3-蒈烯,占总挥发性成分的42.14%。结论：升麻生品和炮制品挥发性成分总离子流图的峰形较相似,但化学成分差异较大,含量大不相同。本研究可为升麻药材研发和综合利用提供科学依据。     

参芪益智散挥发性成分分析

摘 要 目的： 分析参芪益智散的挥发性成分。方法: 顶空固相微萃取法（HS SPME）结合气质联用技术（GC MS）分析复方粉末中的挥发性成分;水蒸气蒸馏法（SD）结合GC MS对复方挥发油进行分析鉴定。结果: HS SPME GC MS法从复方混合物粉末中检测出挥发性成分117种,鉴定出70种,相对含量占总挥发性成分的94.46%,其中含量最高的为β 雪松烯（19.31%）,其次为衣兰烯（15.56%）、β 细辛醚（7.36%）;SD GC MS法从复方挥发油成分中检测出66种,鉴定出43种,相对含量占总挥发性成分的77.41%,其中含量最高的为β 细辛醚（16.73%）,其次为丁香酚甲醚（6.74%）、衣兰烯（5.81%）。结论:参芪益智散挥发性成分主要为β 细辛醚、α 细辛醚、β 雪松烯、衣兰烯、榄香素、芳樟醇等。本研究为参芪益智散挥发性成分分析提供了方法学基础。     

苏合香挥发性化学成分的GC-MS研究

目的:研究苏合香的挥发性化学成分。方法:通过固相微萃取技术提取苏合香的挥发性成分,采用气相色谱-质谱联用技术进行分析鉴定。结果:共鉴定出苏合香28种成分,占总色谱峰面积的90.72%,其中α-蒎烯(15.97%)、莰烯(13.28%)和β-蒎烯(12.82%)的含量较高。结论:本方法简便、高效,可为芳香辛味含挥发性成分药物的成分研究提供参考。     

Investigation of urinary volatile organic metabolites as potential cancer biomarkers by solid-phase microextraction in combination with gas chromatography-mass spectrometry

Background:

Non-invasive diagnostic strategies aimed at identifying biomarkers of cancer are of great interest for early cancer detection. Urine is potentially a rich source of volatile organic metabolites (VOMs) that can be used as potential cancer biomarkers. Our aim was to develop a generally reliable, rapid, sensitive, and robust analytical method for screening large numbers of urine samples, resulting in a broad spectrum of native VOMs, as a tool to evaluate the potential of these metabolites in the early diagnosis of cancer.

Methods:

To investigate urinary volatile metabolites as potential cancer biomarkers, urine samples from 33 cancer patients (oncological group: 14 leukaemia, 12 colorectal and 7 lymphoma) and 21 healthy (control group, cancer-free) individuals were qualitatively and quantitatively analysed. Dynamic solid-phase microextraction in headspace mode (dHS-SPME) using a carboxen-polydimethylsiloxane (CAR/PDMS) sorbent in combination with GC-qMS-based metabolomics was applied to isolate and identify the volatile metabolites. This method provides a potential non-invasive method for early cancer diagnosis as a first approach. To fulfil this objective, three important dHS-SPME experimental parameters that influence extraction efficiency (fibre coating, extraction time and temperature of sampling) were optimised using a univariate optimisation design. The highest extraction efficiency was obtained when sampling was performed at 50°C for 60 min using samples with high ionic strengths (17% sodium chloride, w v⁻¹) and under agitation.

Results:

A total of 82 volatile metabolites belonging to distinct chemical classes were identified in the control and oncological groups. Benzene derivatives, terpenoids and phenols were the most common classes for the oncological group, whereas ketones and sulphur compounds were the main classes that were isolated from the urine headspace of healthy subjects. The results demonstrate that compound concentrations were dramatically different between cancer patients and healthy volunteers. The positive rates of 16 patients among the 82 identified were found to be statistically different (P<0.05). A significant increase in the peak area of 2-methyl-3-phenyl-2-propenal, p-cymene, anisole, 4-methyl-phenol and 1,2-dihydro-1,1,6-trimethyl-naphthalene in cancer patients was observed. On average, statistically significant lower abundances of dimethyl disulphide were found in cancer patients.

Conclusions:

Gas chromatographic peak areas were submitted to multivariate analysis (principal component analysis and supervised linear discriminant analysis) to visualise clusters within cases and to detect the volatile metabolites that are able to differentiate cancer patients from healthy individuals. Very good discrimination within cancer groups and between cancer and control groups was achieved.     

顶空气相色谱质谱法检测食品中呋喃的影响因素

目的分析顶空气相色谱-质谱法检测食品中呋喃并对影响因素进行分析,确定最佳的实验条件。方法分析顶空密封加热过程中呋喃和d4-呋喃的泄漏和分解而带来的损失;顶空分析的平衡温度、时间的选择以及加入硫酸铵的作用;比较标准加入法和标准曲线法进行呋喃定量分析结果的差异性。结果顶空分析过程中呋喃和d4-呋喃不会因泄漏和分解而影响其稳定性;选择顶空温度50℃平衡30min,可提高呋喃测定的准确性;加入硫酸铵可提高顶空分析呋喃的灵敏性;标准加入法和标准曲线法是两种等效的定量方法。结论选择d4-呋喃作为内标物,顶空50℃恒温30min后,经气相色谱质谱仪分离扫描,标准曲线法定量,是理想的食品中呋喃检测实验条件。