顶空液液萃取-气相色谱-质谱法用于白术挥发性成分的分析

采用高温顶空液相萃取再转移的方法,对中药白术中挥发性成分进行萃取分离富集,采用顶空液液萃取/气相色谱-质谱(HS-LP-LPE/GC-MS)联用法进行测定,并与传统水蒸汽蒸馏法(SD)提取的挥发性成分进行对比。对各种测定条件和影响因素进行了考察,最佳萃取条件为:1.0 mL PEG 400为高温萃取剂,样品用量1.2 g,萃取温度120℃,萃取时间60 min,再将萃取剂用1.0 mL正己烷进行反萃取后进行GC-MS分析;采用HS-LP-LPE/GC-MS鉴定了33个组分,占总组分含量93.18%;SD鉴定了31个组分,占总组分含量97.12%。两种方法共同检测到的组分有29个,均以苍术酮(Atractylone)含量最高。结果表明,两种方法所提取的组分基本相同,可用于白术挥发性成分的测定。     

顶空-固相微萃取法与水蒸气蒸馏法提取沙棘挥发油组分的比较研究

优化了顶空-固相微萃取法(HS-SPME)提取沙棘挥发性成分的条件,并采用气相色谱-质谱联用技术(GC-MS)分别对HS-SPME法和水蒸气蒸馏法(SD)的提取物进行分析。结果显示,在萃取温度为70℃,萃取时间为50 min,解吸时间为7 min,平衡时间为20 min条件下,HS-SPME法鉴定出76种组分,占挥发性物质总量的90.19%,主要成分为酯类、醛类和酮类;而SD法提取物共鉴定出56种组分,占挥发性物质总量的91.98%,主要成分为酯类。2种方法共有组分为20种。两种方法提取的沙棘挥发油组分的种类及含量差异较大,HS-SPME法更适合沙棘挥发性组分的快速检测。     

超临界CO2萃取柚子叶挥发油的研究及GC-MS分析

采用超临界CO2萃取技术提取柚子叶的挥发性成分,以挥发油得率为衡量工艺参数的指标,通过正交试验法考察超临界CO2萃取过程中萃取温度、萃取压力、CO2的流量及萃取时间4个因素对柚子叶挥发油得率的影响。结果表明20MPa、萃取温度45℃、CO2流量7kg·h-1、萃取时间120min为最佳工艺。通过GC-MS对挥发油进行分析,从柚子叶挥发油中分离出144个组分,鉴定了61种成分,占化合物检出总量的90.4%。     

不同方法提取香椿芽挥发油的比较研究

采取超-临界CO2萃取、乙醚超声波萃取、乙醚微波萃取和微波水蒸气萃取4种方法提取香椿芽挥发油,利用气相色谱.质谱联用技术,分析了挥发油的化学组成,并进行了比较.结果表明:4种提取方法得到的挥发油的化学组分存在差异,其中含有20种相同的化合物,一种未鉴定,其余19种主要是相对分子质量为204.19的倍半萜类化合物和相对分子质量在240～280之间的化合物,但各组分的含量有差异.     

GC–MS法分析茵陈挥发油成分

采用水蒸气蒸馏法提取茵陈中挥发性成分挥发油,用气相色谱–质谱联用技术(GC–MS)对茵陈挥发油成分进行分析鉴定,并采用峰面积归一化法测定其相对含量。共检出52种挥发性成分,鉴定了其中31种主要挥发性成分,含量较高的组分为石竹素(15.27%)、(–)-斯巴醇(6.64%)、石竹烯(4.89%)等。GC–MS法适用于茵陈挥发性成分的定性分析,具有灵敏度高、分析速度快的特点。     

吹扫/捕集-热脱附气质联用法对荷叶挥发油成分的对比分析

采用同时蒸馏萃取提取得到荷叶挥发油, 通过吹扫/捕集-热脱附法(P&T-TD)对上述提取物中挥发性成分进行富集, 以气质联用(GC/MS)进行定性检测, 同时与直接进样GC/MS法分析的成分进行比较. 两种方法成功分离分析出有机酸、酯、醛、醇、酚、烷烃、芳香烃、烯烃以及含氮、硫、氧杂原子的化合物等共计84种成分, 其中P&T-TD GC/MS鉴定出63种有机化合物, GC/MS鉴定出41种有机化合物, 有20种成分共同检出. 对比分析表明: P&T-TD GC/MS的吹扫/捕集-热脱附过程能富集各种组分, 相比GC/MS分析, 可以鉴定出微量成分及更多挥发性和半挥发性成分, 在精油等挥发性成分的分析检测中使用优势明显.     

超声辅助-表面活性剂增强乳化微萃取-气相色谱-质谱法测定薄荷芳香水中的挥发性成分

提出了基于低密度溶剂超声辅助-表面活性剂增强乳化微萃取-气相色谱-质谱法测定薄荷芳香水中的挥发性成分。优化的试验条件如下:1萃取剂为甲苯;21mg·L-1吐温80溶液的用量为30μL;3超声时间为1min。在气相色谱分离中用DB-5石英毛细管柱为固定相,在质谱分析中采用全扫描检测模式。方法用于薄荷样品的分析,薄荷芳香水中共鉴定出20种挥发性成分,薄荷挥发油中共鉴定出30种挥发性成分,其中所含的主要成分基本一致。     

顶空固相微萃取-气相色谱-质谱法用于白术中挥发性成分的分析

采用顶空固相微萃取-气相色谱-质谱法(HS-SPME-GC-MS)分离鉴定了白术中的挥发性成分,并与采用传统的水蒸气蒸馏法(SD)提取的挥发性成分进行了比较。实验中筛选了固相微萃取纤维头,优化了SPME的操作条件。样品在70 ℃下平衡30 min后,用65 μm聚二甲基硅氧烷-二乙烯基苯(PDMS-DVB)纤维头对白术样品顶空吸附30 min,于250 ℃下解吸4 min, 然后采用GC-MS对解吸物进行分离鉴定;采用HS-SPME-GC-MS鉴定出41种组分,占总峰面积的90.81%;采用SD-GC-MS鉴定出31个组分,占总峰面积的88.19%,且采用SD所提取的组分基本上都被固相微萃取所提取。结果表明, HS-SPME可取代耗时的SD用于白术中挥发性物质的提取。     

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%)。     

烟用香精中风味成分的提取条件的优化与测定

分别采用溶剂萃取、同时蒸馏萃取、固相微萃取和水蒸汽蒸馏等4种方法提取烟用香精B3样品中的挥发性和半挥发性风味成分,并采用信息量和重现性两个指标考察最优提取方案。正己烷溶剂萃取法具有相对较高的信息量和理想的重现性。通过GC和GC-MS进行定性定量分析,共鉴定了34种成分,定性了的成分占总成分的85．4％。     

微波辐射法提取柚皮、橙皮的挥发油

The essence oil of citrus grandis peel and orange peel was extracted by the microwave method in this article.The results show that the best condition of extracting is when 100 g peel is extracted at 360 W with n-hexane for 50 s,the obtained rate of pomelo oil is 1.73% and orange oil is 0.65%.     

Comparative analysis of headspace volatiles of Chinese Rosa rugosa

The floral headspace compounds of Chinese Rosa rugosa germplasms that were isolated by an automated headspace sampler with built-in trap, and followed by gas chromatography-mass spectrometry for identification and quantification. Up to 33 volatile compounds were identified from the 23 rose germplasms, including nine alcohols, five esters, three alkanes, 10 terpenes, three aldehydes, two ketones, and one ether. The main floral components identified were 2-phenylethanol, β-citronellol, ethanol, and n-hexane. 'xizi', 'miaofengshan', 'xiangciguo', and 'tangbai' contained the highest amounts of 2-phenylethanol at 84.66 μg·g?1, β-citronellol at 70.98 μg·g?1, ethanol at 83.87 μg·g?1, and n-hexane at 18.23 μg·g?1, respectively. 'Rongchengyesheng', 'tanghong', 'xizi', 'miaofengshan', and 'baizizhi' could be considered good materials for extracting rose oil and breeding new cultivars.     

汽油中有机硫化物的酸富集和结构分析

石油中发现的硫化物已超过250种，其中约有1／4存在于汽油中。由于汽油中每种硫化物的含量都很低，又有十分复杂的烃组分和含氮组分的干扰，单纯使用仪器方法对汽油中的有机硫化物进行结构分析是十分困难的。通常的做法是对汽油样品进行预处理，使硫化物从混合烃体系中分离出来，再通过仪器和相应标样进行类型分析或结构鉴定。目前研究者在此方面做了很多工作，花瑞香等用29种硫化物标样，采取GC／SCD辅以选择性化学反应对汽油馏分的硫化物形态分布研究。     

Hydrodistillation-headspace solvent microextraction, a new method for analysis of the essential oil components of Lavandula angustifolia Mill

A new method involving concurrent headspace solvent microextraction combined with continuous hydrodistillation (HD-HSME) for the extraction and pre-concentration of the essential oil of Lavandula angustifolia Mill. into a microdrop is developed. A microdrop of n-hexadecane containing n-heptadecane (as internal standard) extruded from the needle tip of a gas chromatographic syringe was inserted into the headspace above the plant sample. After extraction for an optimized time, the microdrop was retracted into the syringe and injected directly into a GC injection port. The effects of the type of extracting solvent, sample mass, microdrop volume and extraction time on HD-HSME efficiency were investigated and optimized. Using this method, thirty-six compounds were extracted and identified. Linalool (32.8%), linalyl acetate (17.6%), lavandulyl acetate (15.9%), alpha-terpineol (6.7%) and geranyl acetate (5.0%) were found to be the major constituents. To the best of our knowledge this is the first report on the use of continuous headspace solvent microextraction coupled with hydrodistillation for investigation of essential oil components.     

Ionic liquid-based microwave-assisted extraction of essential oil and biphenyl cyclooctene lignans from Schisandra chinensis Baill fruits

Ionic liquid-based microwave-assisted extraction (ILMAE) has been successfully applied in extracting essential oil and four kinds of biphenyl cyclooctene lignans from Schisandra chinensis Baill. 0.25 M 1-lauryl-3-methylimidazolium bromide ionic liquid is selected as solvent. The optimum parameters of dealing with 25.0 g sample are 385 W irradiation power, 40 min microwave extraction time and 1:12 solid-liquid ratio. The yields of essential oil and lignans are 12.12±0.37 ml/kg and 250.2±38.2 mg/kg under the optimum conditions. The composition of the essential oil extracted by hydro-distillation, steam-distillation and ILMAE is analyzed by GC-MS. With ILMAE method, the energy consumption time has not only been shortened to 40 min (hydro-distillation 3.0 h for extracting essential oil and reflux extraction 4.0 h for extracting lignans, respectively), but also the extraction efficiency has been improved (extraction of lignans and distillation of essential oil at the same time) and reduces the environmental pollution. S. chinensis materials treated by different methods are observed by scanning electronic microscopy. Micrographs provide more evidence to prove that ILMAE is a better and faster method. The experimental results also indicate that ILMAE is a simple and efficient technique for sample preparation.     

High-performance liquid chromatographic separation of the fat-soluble vitamins in cod liver oil and feeds

A MicroPak-CN column with a methylene chloride—chloroforms-n-hexane (3:2:15) mobile phase separates the fat-soluble vitamins in cod liver oil and formulated feed. Powdered feed samples are dissolved in n-hexane—chloroform—ethanol (6:3.5:0.5) and centrifuged before injection. The oil is dissolved in the extraction solvent or mobile phase before injection. The naturally occurring vitamins are identified from their absorption spectra by stopped-flow spanning of the individual vitamins.     

Comparative study on the antioxidant activities of the different extracts and the composition of the oil extracted by n-hexane from Iranian Vitex pseudo-negundo

Antioxidant activities of different extracts obtained from the aerial parts of Vitex pseudo-negundo from Kashan, central Iran, were evaluated for the first time in this study using β-carotene/linoleic acid and scavenging of free-radical (DPPH) assays. Water extract showed the highest activity in both assays. GC-MS analysis of the oil extracted by n-hexane revealed 46 compounds with trans-β-farnesene being the main component. Several new compounds, not reported in the previous literature, were identified in the essential oil of this chemo-type.     

超临界和近临界条件下Fischer Tropsch合成研究：溶剂的影响

研究了超临界和近临界条件下费托合成过程中溶剂对反应行为的影响。反应在固定床反应器中进行，催化剂为Co/SiO2，所选择的溶剂有两类：纯溶剂（正戊烷和正己烷）和混和溶剂（由正己烷和少量的C5~10烃组成）。结果表明,正己烷分压对CO转化率影响很小，但是产物中1 烯烃含量随正己烷分压增加而增加，超临界条件下1 烯烃含量明显高于非临界条件下。溶剂的种类对CO转化率、CH4和CO2选择性以及产物炭分布影响不大。这一结果表明为了减少溶剂用量，对含有适量轻组分（C5~10）的正己烷溶剂进行循环使用是可行的。结果同时表明与正己烷相比，混和溶剂（25%正己烷和75%正葵烷）具有较高的1 烯烃选择性。     

西洋参中挥发油化学成分的分析

利用气相色谱－质谱－计算机联用装置分析吉林栽培西洋参挥发油中的化学成分及相对含量。由于没有按照常规的乙醚提取，而紧 ８０％的甲醇提取，因此得到的挥发油成分及含量与文献报道有很大的差别，共鉴定出２３种化合物，其中醌类及酸类约占总挥发油含量的６５％，为该部分挥发油的主要成分。     

稠油催化裂解前后咔唑类化合物的变化及其催化降黏机理的研究

在稠油族组成分离中,采用低毒试剂正己烷、二氯甲烷、无水乙醇及其混合溶剂,将反应前后已除去沥青质的稠油分离为饱和烃、芳烃和含氮化合物。优化并确立了各步分离条件,用GC-MS对各组分进行检测,了解水热催化裂解降黏前后各组分的变化,剖析了胶质中咔唑类化合物的变化。并结合¹HNMR、元素分析等分析手段,证明稠油经水热催化裂解反应后,重质组分中的含氮组分发生了变化,生成了部分咔唑类化合物, 同时,重质组分的组成和结构也发生了一定程度的改变,其超分子结构在一定程度上遭到破坏,生成二环、三环低环数芳烃和小分子量直链烃。这些变化使得稠油黏度降低。