树兰花净油化学成份的研究

用气相色谱-质谱-数据系统联用技术以及红外和核磁共振光谱分析了树兰花净油的化学成份。其萜烯部分除已报道过的(王古)(王巴)烯、丁香烯、蛇麻烯、榄香烯之外,还发现有a-橙椒烯、β-橙椒烯、双环榄香烯、β-檀香烯、γ-木罗烯、金合欢烯、α-木罗烯、β-没药烯、β-荜澄茄烯、γ-荜澄茄烯、δ-荜澄茄烯、γ-榄香烯、白菖烯、甜旗烯等倍半萜烯;而含氧部分的主要成份是茉莉酮酸甲酯和蛇麻烯环氧物Ⅱ;此外还发现有蛇麻二烯酮、蛇麻烯环氧物Ⅰ、蛇麻烯-7醇、丁香烯环氧物、T-荜澄茄醇、δ-荜澄茄醇、表-橙椒醇、橙椒醇、芳萜醇等。     

树兰花水蒸汽蒸馏挥发油的成份研究

继树兰花净油的分析之后,我们用气相色谱-质谱-数据系统联用技术以及红外和核磁共振光谱分析了树兰花水汽蒸馏挥发油的化学成份。发现其萜烯部分有:α-橙椒烯、(王古)(王巴)烯、丁香烯、双环榄香烯、蛇麻烯、β-檀香烯、γ-木罗烯、双氢姜黄烯、α-木罗烯、β-没药烯、白菖烯、甜旗烯。其含氧部分有甲基庚烯酮、2-乙基己醇-1、橙做醇、表-橙椒醇、丁香烯环氧物、乙酸苄酯、苄醇、蛇麻二:烯酮、芳萜醇、表-苦本醇、蛇麻烯环氧物Ⅰ、蛇麻烯环氧物Ⅱ、T-荜澄茄醇、蛇麻醇、δ-荜澄茄醇、荜澄茄烯醇、丁香二烯醇、蛇麻烯-7醇和茉莉酮酸甲酯。     

火炬松挥发物的固相微萃取-气相色谱/质谱法分析

采用固相微萃取(SPME)技术,结合气相色谱/质谱(GC-MS)分析了火炬松枝条和针叶中的挥发性化合物,共鉴定了30种化学成分。其中枝条中分离鉴定出21种挥发性成分。主要成分为α-蒎烯、β-蒎烯、β-月蒎烯、反式-石竹烯、β-杜松烯、大根叶烯-D;针叶中分离鉴定出24种挥发性成分,主要成分为α-蒎烯、β-蒎烯、β-月桂烯、β-水芹烯、异长叶烯、反式-石竹烯、α-律草烯、大根叶烯-D、双环吉马烯和双环榄香烯。     

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。     

广西产湿地松松针挥发性成分的提取及分析

采用水蒸气蒸馏法提取湿地松针叶挥发油的油相部分,用乙醚萃取法提取蒸馏残液中的水溶性挥发性组分,利用气相色谱-质谱联用分析比较二者的化学成分。湿地松挥发油油相部分的得油率为0.277%,共分离出86个色谱峰,鉴定了其中的49种化合物,占总含量的92.12%,油相部分的主要成分有β-蒎烯（14.29%）、吉马烯（12.87%）、α-蒎烯（6.79%）、β-石竹烯（6.15%）、α-石竹烯（1.58%）;水溶性部分的得油率为0.0682%,鉴定了其中的6种化合物,占水溶性部分总量的60.72%,α-松油醇（24.61%）为水溶性部分的主要成分。由于增加了水溶部分精油的提取,湿地松松针挥发油总的产油率提高到0.3452%,提高率达24.62%。     

气相色谱/质谱法分析柏树叶挥发油的化学成分

采用水蒸气蒸馏技术提取了3种柏树叶的挥发油,经气相色谱/质谱分析,共分离和鉴定了64种化学成分,其主要成分为萜烯类,其他成分为烷烃类、醇类、酚类和酯类等。其中圆柏树叶中分离鉴定出33种挥发性成分,主要萜类为桧烯(20.99%)和柠檬烯(19.78%);中山柏树叶中分离鉴定出37种挥发性成分,主要为α-蒎烯(10.39%)、桧烯(11.19%)和δ-3-蒈烯(8.88%);龙柏树叶中分离鉴定出37种挥发性成分,主要为柠檬烯(24.56%)和β-月桂烯(8.04%)。分离鉴定出3种柏树叶的共有成分14种。     

木豆精油化学成分研究

用水蒸汽蒸馏法从木豆的叶和嫩枝中提出挥发油,并用交联毛细管柱气相色谱/质谱/计算机(GC/MS/MSD)联用技术测定木豆精油的化学成分。从中鉴定出23种化合物,主要成分为:菖蒲烯,β-芹子烯,α和β-Cuaiene,α-himachalene,苯甲酸苄酯和雅槛兰树油烯。     

香樟树叶挥发油的化学成分研究

用同时蒸馏萃取法(SDE)和气相色谱-质谱连用技术(GC-MS)对香樟树叶挥发油成分进行了分离分析,共鉴定出98种化合物。其中主要成分为樟脑与β-芳樟醇(24.099%)、桉油醇(15.723%)、α-松油醇(11.204%)、石竹烯(4.957%)、蛇床-6-烯-4-醇(5.724%)、β-水芹烯(3.394%)等。     

超临界CO2萃取石菖蒲有效成分的GC-MS分析

采用超临界ＣＯ２流体萃取技术从石菖中萃取分离挥发油,用气相色谱－质谱联用技术测定其化学成分,从中鉴定出２６种成分,并测定了其相对含量,主要成分为：顺－细辛脑、反－细辛脑、绿叶烯、石竹烯、蛇麻烯、甲基丁子香酚、榄香纱,顺－罗勒烯等。     

固相微萃取结合气-质联用分析侧柏叶中的挥发性成分

以产自河北的侧柏叶为原料,采用四种固相微萃取纤维对其中的挥发性成分进行提取,用气质联用进行分析,共分离出112种成分,采用质谱与保留指数进行定性,鉴定出87种成分(四种萃取纤维的提取物中都鉴定出的成分有59种),其中烯烃类51种(以单萜和倍半萜为主),烷烃类4种,芳香烃类3种,醇类18种,醛酮类3种,酯类4种,醚类3种,吡嗪类1种;另外采用质谱初步定性出12种。采用面积归一化法确定了它们的相对含量,含量较高的有(1R)-(+)-α-蒎烯、(+)-3-蒈烯、D-柠檬烯、β-水芹烯、δ-松油烯、β-榄香烯、石竹烯、顺式-罗汉柏烯、葎草烯、大根香叶烯D、δ-杜松烯、柏木脑等。对比所得结果可以发现,CAR/PDMS(85μm)的萃取纤维对侧柏叶中挥发性成分的提取效果较好。     

气相色谱-质谱法分析橡苔浸膏中的挥发性化学成分

 用挥发油提取器提取橡苔浸膏中的挥发油,利用气相色谱-质谱法(GC-MS)分析了其中的化学成分,采用GC峰面积归一化法定量,鉴定出24种化合物,共占挥发油总量的83%以上     

山楂挥发性化合物的气相色谱-质谱分析

采用蒸馏－萃取法收集山楂果的挥发性化合物,通过气相色谱及气相色谱／质谱分析,鉴定了３２种化合物,占总峰面积的６１％～６８％。其中主要的１０种化合物是顺－３－己烯醇、顺－３－乙酸己烯酯、α－萜品醇、糠醛、己醇、乙酸己酯、壬醛、柠檬醛、３－戊烯－２－酮,反－２－癸烯醛等。     

High-throughput analysis of bergamot essential oil by fast solid-phase microextraction-capillary gas chromatography-flame ionization detection

The advantages of using a narrow-bore column in headspace solid-phase microextraction-gas chromatographic (HS-SPME-GC) analysis are investigated. An automated rapid HS-SPME-GC method for the determination of volatile compounds in a complex sample (bergamot essential oil) was developed. A low-capacity (7 microm) SPME fibre was employed, enabling a short equilibration time (15 min). The absorbed volatile compounds were then separated in 12.5 min on a 10 m x 0.1 mm I.D. capillary. The fast GC method was characterized by relatively moderate GC parameters (head pressure: 173 kPa; temperature program rate: 12 degrees C/min). The employment of the low-capacity fibre also suited the reduced sample capacity of the capillary employed, hence column overloading was avoided. Analytical repeatibility was determined in terms of retention times (maximum RSD: 0.32%) and peak areas (maximum RSD: 9.80%). The results obtained were compared to those derived from a conventional HS-SPME-GC (a 30 microm SPME fibre and 0.25 mm I.D. capillary were used) application on the same sample. In this respect, a great reduction of analytical time was obtained both with regard to the conventional SPME equilibration and GC run times, which both required 50 min. Peak resolution was altogether comparable in both applications. Although a slight loss in terms of sensitivity was observed in the rapid approach (generally within the 25-50% range), this did not impair the detection of all peaks of interest. Finally, the selectivities of the 30 and 7 microm fibres were evaluated and, as expected, these were in good agreement.     

气相色谱-质谱法测定大蒜挥发油的组成

采用改进的水蒸汽蒸馏法从山东金乡大蒜中提取挥发油。实验确定了气相色谱-质谱法分析大蒜油的条件,并对大蒜挥发油的化学成分进行了定性分析,共鉴定出20种物质。用峰面积归一化法对各物质的相对含量进行了测定,结果表明含硫化合物约占挥发油总成分的95%以上,其中含量最高的是大蒜新素,约占挥发油总量的三分之一。对低温储藏半年的挥发油进行分析的结果表明样品在低温下可稳定存放。     

气相色谱-质谱联用测定柴油机排气微粒中的可溶性有机组分

采用气相色谱-质谱联用技术(GC/MS)对柴油机排气微粒中的可溶性有机组分(SOF)进行了分离分析。SOF分析液样品采用超声提取法制取。GC条件为:SE-50型石英毛细管色谱柱(30 m×0.2 mm i.d.×0.2 μm）;程序升温：初始温度100 ℃,恒温2.0 min,以4.0 ℃/min升至160 ℃,再以8 ℃/min升至250 ℃,恒温31.75 min;汽化室温度260 ℃;载气为氦气,柱头压力45 kPa;进样量1 μL。MS条件为:电子轰击离子源,电子轰击能量70 eV;倍增器电压18     

Fast capillary GC using a low thermal mass column oven for the determination of residual solvents in pharmaceuticals

A low thermal mass column oven was used for fast capillary GC analysis (high throughput) of residual solvents in pharmaceutical products. A dedicated capillary column, 20 m L x 180 microm ID x 1 microm DB-624 was programmed from 35 degrees C (30 s) to 150 degrees C at 100 degrees C/min and to 250 degrees C (30 s) at 200 degrees C/min, resulting in a total GC cycle time of less than 4 min. Complete separation of a target 20-component mixture was achieved, while method performance in terms of repeatability, sensitivity, and linearity was maintained in comparison to the generic method currently applied in our laboratories.     

气相色谱-质谱法测定姜黄挥发油化学成分

采用水蒸气蒸馏法提取姜黄挥发油,用气相色谱－质谱联用技术分离和鉴定姜黄挥发油的化学成分。经计算机ＮＢＳ谱库检索,发现姜黄挥发油中至少有１５个峰,鉴定出α－姜黄烯、α－姜烯、桉叶油素和球姜酮等１５种组分;另外还有１－（３－环戊基醛）－２,４－二甲基苯、β－倍半水芹烯、大根香叶酮、大根香叶烷、顺双环［３,３,１］酮－２－烯－９－醇等成分。姜黄挥发油中主要成分为α－姜黄烯。     

Simultaneous determination of some active ingredients in cough and cold preparations by gas chromatography, and method validation

A simple and rapid gas chromatographic (GC) method has been developed for the simultaneous determination of combinations of acetaminophen, phenylpropanolamine hydrochloride, guaifenesin, pseudoephedrine hydrochloride, caffeine, chlorpheniramine maleate, and dextromethorphan hydrobromide in cough and cold tablets and syrups. After extraction of the analyte with alkaline ethyl acetate, 2 microL extract was injected (splitting ratio of 50:1) into a gas chromatograph equipped with a CBP1-M25-025 fused silica capillary column (25 m x 0.22 mm; film thickness, 0.25 microm). The column temperature was held at 150 degrees C for 5 min, increased to 175 degrees C at 3 degrees C/min, and increased to 270 degreesC at 10 degrees C/min. The temperatures of the flame ionization detector and injector were maintained at 300 degrees C. The GC method is inexpensive, rapid, accurate, and precise, and thus it can be used for routine analysis of tablet and syrup preparations in quality control laboratories of pharmaceutical companies.     

超临界CO2流体萃取法与水蒸气蒸馏法提取荆芥穗挥发油化学成分的研究

采用超临界CO2萃取法(SFE)与水蒸气蒸馏法(SD)从荆芥穗中提取挥发油。采用SE-54毛细管柱进行分析,用气相色谱-质谱法对挥发油中各种化学成分进行鉴定,用归一化法测定各组分的含量。色谱条件:SE-54毛细管柱 (30 m×0.25 mm i.d.,0.25 μm),柱温50 ℃(3 min)5 ℃/min180 ℃(2 min)10 ℃/min260 ℃(50 min);分流进样,分流比1∶50;进样口温度280 ℃。在采用超临界CO2萃取法提取的挥发油中共鉴定出54种成分,其主要成分为长叶薄荷酮、薄荷酮、亚油酸氯化物等;在水蒸气蒸馏法提取的挥发油中共鉴定出39种成分,其主要成分为长叶薄荷酮、薄荷酮、柠檬烯等。超临界法较水蒸气法更加稳定可靠,重现性好,适用于中药挥发油的化学成分分析。     

气相色谱-质谱联用分析花椒挥发油的成分

 采用气相色谱 质谱联用技术对陕西富平产花椒挥发油的成分进行了分析 ,分离出了 17个峰 ,鉴定出了相对峰面积大于 1 0 %的组分共 16个 ,用峰面积归一化法定量测定了已确定组分的相对含量 ,其占挥发油总质量的95 %以上。