GC-MS analysis of volatile compounds of Perilla frutescens Britton var. Japonica accessions: morphological and seasonal variability

Objective: To investigate the composition of volatile compounds in the different accessions of Perilla frutescens(P. frutescens) collected from various habitats of China and Japan. Methods: In the present study, the essential oil from the leaves of P. frutescens cultivars from China and Japan was extracted by hydro-distillation and the chemical composition and concentration of the volatile components present in the oils were determined by gas chromatography–mass spectrometry(GC–MS) analysis. Results: Among the volatile components, the major proportion was of perilla ketone, which was followed by elemicin and beta-caryophyllene in the Chinese Perilla cultivars. The main component in the oil extracted from the Japanese accessions was myristicin, which was followed by perilla ketone and beta-caryophyllene. We could distinguish seven chemotypes, namely the perilla ketone(PK) type, perilla ketone, myristicin(PM) type, perilla ketone, unknown(PU) type, perilla ketone, beta-caryophyllene, myristicine(PB) type, perilla ketone, myristicin, unknown(PMU) type, perilla ketone, elemicine, myristicin, beta-caryophyllene(PEMB) type, and the perilla ketone, limonene, betacryophyllene, myristicin(L) type. Most of the accessions possessed higher essential oil content before the flowering time than at the flowering stage. The average plant height, leaf length, leaf width of the Chinese accessions was higher than those of the Japanese accessions. Conclusion:The results revealed that the harvest time and geographical origin caused polymorphisms in the essential oil composition and morphological traits in the Perilla accessions originating from China and Japan. Therefore, these chemotypes with desirable characters might be useful for industrial exploitation and for determining the harvest time.

基于HS-GC-IMS分析爆珠香精挥发性风味成分差异

采用顶空气相色谱-离子迁移谱(HS-GC-IMS)技术,对不同清新玫瑰爆珠样品中的香精挥发性成分进行鉴定,并通过感官评价,结合主成分分析(PCA)、偏最小二乘判别分析(PLS-DA)、偏最小二乘回归法(PLSR)等多元统计方法识别判定不同样品的主要风味成分差异。结果表明:①感官评价显示该爆珠样品风格特征主要以花香、果香、木香为主,并辅以青香、甜香与酒香香韵,不同样品在花香、果香属性上呈显著差异(p<0.05);②GC-IMS非靶向定性出样品中22种主要的挥发性风味组分,其中醇类8种、酯类3种、酮类3种、醛类3种、烯烃类3种、酸类1种、吡嗪类1种,且指纹图谱直观显示出挥发性较强的醇类、酯类等香气化合物在样品间差异明显;③PCA、PLS-DA能对不同样品进行有效区别,并筛选出10个特征差异组分(VIP>1),PLSR得出样品感官差异主要与2-甲基丁酸乙酯、丁酸乙酯、环己酮、苯乙酮、辛醛、正丙醇和芳樟醇有关。该方法可有效区分不同清新玫瑰爆珠样品,其判定结果与感官评价结果一致,具有准确可靠、可视化强等特点,能够为烟用爆珠产品感官质量快速检验提供技术支持。

基于GC-IMS技术分析五种市售不同工艺油莎豆油理化品质与风味差异

为研究市售不同工艺油莎豆油理化品质与风味的差异性,采用气相离子迁移谱(Gas Chromatography-Ion Mobility Spectroscopy,GC-IMS)技术结合主成分分析法对比不同工艺(物理压榨、热榨、亚临界萃取、高压冷榨和冷榨工艺)油莎豆油挥发性化合物之间的差异性。GC-IMS结果显示,不同工艺油莎豆油中共鉴定出76种挥发性化合物,其中包括酯类12种、醇类16种、醛类29种、酮类9种、酸类5种、呋喃类3种、吡嗪类1种、硫类1种。热榨组醛类、酯类和呋喃类物质相对含量较高(53.54%,13.06%,5.41%)。不同工艺油莎豆油风味差异性主要来源于四种关键风味物质:1-烯-3-辛醇、壬醛、(E)-2-辛烯醛和己醛。主成分分析(Principal Component Analysis,PCA)结果表明PC1和PC2分别为48.7%和30.1%,累计差异贡献率为78.8%,不同工艺油莎豆油风味物质差异显著,能够对不同工艺油莎豆油良好区分。Pearson相关性分析结果表明不同工艺油莎豆油b*值与酸价、过氧化值、p-丙二醛值和1-烯-3-辛醇之间呈显著正相关(0.57<r<0.88,P<0.05)。本研究结对市售油莎豆油生产加工、理论研究和质量检测等领域具有一定的参考价值。

基于HS-GC-IMS分析陇南主栽品种初榨橄榄油的风味特征成分

旨在为我国甘肃陇南产区初榨橄榄油(VOO)的快速鉴别以及工业生产过程中的风味品质评价提供数据支撑和理论依据,采用HS-GC-IMS技术对甘肃陇南主栽品种莱星(LX)、佛奥(FO)、科拉蒂(KLD)、皮削利(PXL)、鄂植8号(EZ8)以及LX与KLD的混合品种(HH)6种VOO中的风味特征成分进行定性和差异分析。结果表明:6种VOO中共检测出39种风味特征物质,定性出22种,其中醛类(9种)、酮类(5种)化合物为主要的风味特征成分,此外还包括酯类(3种)、醇类(3种)、萜烯类(1种)和呋喃类(1种)等物质;6种VOO中含有的风味特征物质均存在不同程度的差异,其中,LX、KLD和HH中的风味特征物质较为相似,其2-甲基丁醛、3-甲基丁醛、(E)-2-戊烯醛、辛醛和2-正戊基呋喃含量较高,FO中的正戊醇、正己醛和3-戊酮含量较高,PXL中的(Z)-3-己烯乙酸酯、α-松油烯、2-己酮的含量较高,EZ8中的乙酸乙酯含量最高,HH中的2-丁酮、丙酮、(E)-2-庚烯醛的含量较高。综上,采用HS-GC-IMS可以有效检测VOO中的风味特征物质,定性出的风味特征物质可作为区分6种VOO的依据之一。

基于柱前衍生GC-MS法比较不同工艺制备黄精的氨基酸含量

建立了柱前衍生GC-MS法测定黄精中15种氨基酸含量的方法。测定经不同工艺制备的黄精鲜品、干品及炮制品样品中氨基酸的含量,并运用多元数据统计对这3种不同黄精样品中的氨基酸进行综合分析。结果表明:三种黄精制品中的15种氨基酸在33min内有良好的分离效果,在线性范围内线性关系良好(r:0.9983〜0.9999),平均加样回收率为95.66%〜105.55%(n=6)。说明该方法能准确测定黄精中多种氨基酸的含量,且黄精鲜品氨基酸含量明显高于干品及炮制品。聚类及正交偏最小二乘法-判别分析结果表明,黄精鲜品、干品和炮制品可以明显聚为不同三类,说明上述三种黄精制品的氨基酸含量有明显差异性,并筛选出赖氨酸、组氨酸、甘氨酸和络氨酸作为区分黄精鲜品、干品和炮制品的标志物。

CS_2 extraction and FTIR & GC/MS analysis of a Chinese brown coal

The abundance of low-rank coals in China, such as bituminous and brown coals, makes studies of their composition and structure of great significance to both coal chemistry research and for efficient utilization of the coal. We describe how a Chinese brown coal was ultrasonically extracted with carbon disulfide (CS2) and the raw and extracted coals were characterized by Fourier Transform Infrared Spectroscopy (FTIR). The corresponding extract was analyzed with a coupled gas chromatograph mass spectrometer (GC/MS). The FTIR analysis shows a great abundance of amidocyanogen, carbonyl, aromatic and hetero aromatic rings and single carbon-heteroatom bonds. This suggests the possible occurrence of compounds like alcohols, phenols, amines, esters, carboxylic acids, ethers, aromatics or heteroaromatics. The GC/MS analysis of the CS2 extract detected 62 compounds, among which the non-polar ones were of lower abundance while the polar ones were in higher abundance and were structurally diverse. This demonstrates the compositional and structural complexity of Shengli coal.

Chemical composition, antioxidant activity and GC-MS analysis of juice and peel oil of grapefruit varieties cultivated in India

Citrus family especially Grapefruit,has attained considerable attention due to the presence of a number of essential components that have cardiovascular and anti-hypertensive properties.The juice and essential oil extracted from eight recently released grapefruit cultivars were used to study physicochemical and antioxidant properties.The total soluble solids(TSS),titratable acidity(TA) and pH of juice samples extracted from various grapefruit varieties differed significantly.The refractive index,specific gravity and optical rotation values for the oil varied from 1.473 to 1.396,0.863 to 0.847 and +93 to +86,respectively.The percent 2,2-diphenyl-1-picrylhydrazyl radical activity(% DPPH activity) and ferric reducing antioxidant power(FRAP) values for grapefruit juice and peel oil varied from 24.06 to 18.79,2.91 to 1.44 mmol g^–1 and 84.87 to 74.73,7.76 to 5.73 mmol g^-1,respectively.There were significant differences in physicochemical,antioxidant properties and volatile profiles of extracted juice and oil.The oil exhibited higher DPPH and FRAP values than the juice.Among different components identified which accounted for over 99% of the volatile fraction,limonene,myrcene,and benzopyran were major components in all oil samples.

GC-MS analysis,determination of total phenolics,flavonoid content and free radical scavenging activities of various crude extracts of Moringa peregrina(Forssk.) Fiori leaves

Objective:To perform phytochemical screening,estimate total phenolics,flavonoids and to evaluate antioxidant potential of Moringa peregrina(M.peregrina) leaves.Methods:The dried powdered leaves of M.peregrina(150 g) were extracted exhaustively by Soxhlet with ethanol and then fractionated into hexane,chloroform,ethy alacetate and methanol.All the prepared extracts were also analyzed by gas chromatography-mass spectrometry to identify and characterize the chemical compounds present in the crude extracts.Folin- Ciocalteu reagent and aluminium chloride colorimetric methods were used to estimate total phenolic and flavonoid content of extracts.Hydrogen peroxide and 1,1 diphenyl-2-picrylhydrazyl were used to determine in vitro antioxidant activity.Results:Phytochemical analysis of ethanol extract showed presence of major classes of phytochemicals.Gas chromatography-mass spectrometry results revealed presence of 19 phytoconstituents in hexane extract,6 in ethyl acetate and 7 compounds in methanolic extract.Methanol extract was found to contain the highest phenolic content and flavonoids.In vitro antioxidant activities of all crude extracts were significant and comparable with the standard ascorbic acid.Conclusions:Results of this study show that the leaves of M.peregrina are the rich source of phenolic compounds that can play an important role in preventing the progression of many diseases.

基于GC-MS和UPLC-QTOF/MS的灵芝不同生长阶段的成分分析

[目的]探究灵芝(Ganoderma lucidum)不同生长阶段的成分差异。[方法]使用气相色谱-质谱检测法(gas chromatographymass spectrometry,GC-MS)和超高效液相串联四极杆飞行时间质谱法(ultra performance liquid chromatography-quadrupole time-offlight mass spectrometry,UPLC-QTOF/MS)技术,选用ACQUITY超高效液相色谱仪HSS T3色谱柱在Waters超高效液相色谱(ultra performance liquid chromatography,UPLC)系统上对灵芝原基、产孢前和产孢后的子实体进行成分分析与鉴定。[结果]GC-MS共检测到24种成分,其中醛类8种、酯类4种、烃类1种、酸类1种、醇类1种、酮类2种、胺类2种、吡嗪类1种、咪唑类1种、吡咯类1种、呋喃类1种、酚类1种。UPLC-QTOF/MS共检测90种成分,最主要的成分三萜类共有67种,此外还包括脂肪酸类8种、氨基酸及其衍生物类3种、苷类2种、维生素1种、生物碱类2种、有机酸类2种、糖类2种、萜1种、杂萜1种、甾体1种。共有73种成分在原基中检出,其中三萜类成分54种;72种成分在产孢前子实体中检出,其中三萜类成分57种;52种成分在产孢后子实体中检出,其中三萜类成分有42种。[结论]灵芝不同生长阶段成分存在明显差异,本研究结果为灵芝不同时期的化学成分的分析与鉴定,以及化学物谱图的完善提供了基础数据,为相关药理、药效分析提供了有效参考。

Analysis of vapor phase organics in air of Beijing, Langfang and Tianjin by capillary GC and GC/MS

The vapor phase organics (VPOs) in the air of Beijing, Langfang and Tianjin were detected by a capillary gas chromatography and GC/MS during the winter and the summer separately. The tentatively identified compounds include alkanes, cyclic hydrocarbons, alkenes, aromatics, acids, alcohols, aldehydes, ketones, esters, halocarbons and so on. The numbers of VPOs found are 118 in Beijing, 83 in Lang-fang and 65 in Tianjin in the winter, and 56, 39 and 72 in the summer respectively. Based on the data of some representative compounds determined quantitatively by GC and GC/MS, a profile of organic pollution in the air of the three cities is presented.

GC/MS Analysis of Organic Compounds in Hot Water-Extractable Fraction from Shenfu Coal

Shenfu Coal was extracted with hot pure water and slurry was isolated. The concentrated benzene-soluble fraction (CBSF) was analyzed with GC/MS and four types of organic compounds (OCs) were detected: HACOCs,DTEs,DMDT and LCAs. The amount of benzyl benzoate which is the most abundant OC was calculated by an inter-nal standard method with an indicated amount of BP. The broken hydrogen bonds and ether bonds were responsible for the extraction of OCs from the coal .DTEs,DMDT and LCAs are essentially insoluble in water,whereas they are soluble,probably owing to intermolecular interaction of OCs with HACOCs.

多元统计分析结合HS-GC-MS对单粮复合香型白酒挥发性特征差异的分析

采用感官定量描述分析法(SQDA)对A(JA1~JA3)、B(JB1~JB3)、C(JC1~JC3)三组复合香型白酒9个样品的风味结构进行分析,结果表明:三组复合香型白酒在香气评分上差异不显著,粮香、焦香、麦芽香突出,在口感评分上差异显著,A组白酒各维度口感评分高于其他两组。采用顶空-气相色谱质谱联用技术(HS-GC-MS)对3种白酒挥发性化合物组成进行检测分析,共检测到148种挥发性物质。相关性分析结果显示,异丁醛、3-甲基呋喃、二甲基二硫醚、巴豆酸、环氧丙烷、丙烯醛和草酸只在A组白酒中被检测出来,丁酸乙酯在B组白酒中含量最高,JA3中含量偏低,表明3组白酒样品间存在明显的风味物质种类和含量差异。同步结合特征差异代谢物分析挖掘出74个VIP>1的潜在差异代谢物,A vs B组、A vs C组、B vs C组分别有14种、7种、4种化合物呈现极显著性差异(p<0.01),这些含量具有显著差异性的化合物可能与复合香型白酒风味特征的差异具有重要联系。综上所述,本研究采用两种技术协同分析,获得了3种白酒更全面的挥发性风味信息,解析了三组复合香型白酒的风味结构特征及差异,为深入研究复合香型白酒风味形成的机理奠定了基础。

GC–MS analysis of bioactive compounds present in different extracts of an endemic plant Broussonetia luzonica (Blanco) (Moraceae) leaves

Objective: To investigate and characterize the chemical composition of the different crude extracts from the leaves of Broussonetia luzonica(Blanco)(Moraceae)(B. luzonica), an endemic plant in the Philippines.Methods: The air dried leaves were powdered and subjected to selective sequential extraction using solvents of increasing polarity through percolation, namely, n-hexane,ethyl acetate and methanol to obtain three different extracts. Then, each of the extracts was further subjected to gas chromatography–mass spectrometry.Results: Qualitative determination of the different biologically active compounds from crude extracts of B. luzonica using gas chromatography–mass spectrometry revealed different types of high and low molecular weight chemical entities with varying quantities present in each of the extracts. These chemical compounds are considered biologically and pharmacologically important. Furthermore, the three different extracts possess unique physicochemical characteristics which may be attributed to the compounds naturally present in significant quantities in the leaves of B. luzonica.Conclusions: The three extracts possess major bioactive compounds that were identified and characterized spectroscopically. Thus, identification of different biologically active compounds in the extracts of B. luzonica leaves warrants further biological and pharmacological studies.

基于GC-IMS分析新疆不同寄主肉苁蓉挥发性物质

以新疆和田地区‘梭梭’和‘红柳’肉苁蓉为研究对象,采用气相离子迁移色谱(gas chromatography-ion mobility spectroscopy,GC-IMS)分析两种不同寄主肉苁蓉挥发性物质之间的差异。结果表明:GC-IMS共检测出35种挥发性物质,其中定性出27种挥发性物质,包括醛类8种、醇类5种、酯类4种、酮类1种,以醛、醇类物质为主。‘红柳’肉苁蓉和‘梭梭’肉苁蓉挥发性物质差异明显。二者主要差异物质为2-苯基乙醛、苯甲醛、(E)-2-庚烯醛、3-甲硫基丙醛、1-己醛、庚醛、3-甲基-2-丁烯醛、乙酸甲酯、乙酸己酯、1-己醇、乙酰妥英、异丁醇、乙酸乙酯。通过主成分分析可以有效区分两种不同寄主肉苁蓉,PC1和PC2累计方差贡献率达到91%。同时,通过构建挥发性物质聚类热图和指纹图谱等手段,为不同寄主肉苁蓉的鉴定和挥发性物质研究提供理论参考。

Published the papers of GC-MS analysis—Chemical drug

Song Qi, Liu Hu; Gao Shu. Screening and quantitative analysis of volatile markers in the breath of patients with breast cancer Acta Universitatis Medicinalis Anhui, 2010, 45（01） ：76-79.

双酶辅助水蒸气蒸馏法提取肉豆蔻精油及其GC-MS成分分析

采用双酶辅助水蒸气蒸馏法提取广西产肉豆蔻的精油,并通过GC-MS对其进行成分分析。正交实验结果表明,最优提取工艺条件为加酶量2%、酶解pH 4.0、酶解温度40℃,在此条件下,肉豆蔻精油的得率为6.50 mL/100 g。利用GC-MS和保留指数法从精油中鉴定出56种化合物,占精油总量的99.71%,主要成分为肉豆蔻醚(16.60%)、甲基丁香酚(14.78%)、桧烯(13.47%)、(+)-柠檬烯(7.29%)、4-萜烯醇(6.75%)、榄香素(6.62%)、γ-松油烯(4.28%)、反式-甲基异丁香酚(3.73%)、β-蒎烯(3.59%)和黄樟素(3.22%)。

Antibacterial, Antioxidant Activities and GC-MS Analysis of Dichrostachys cinera (L.) Ethanolic Leaves Extract

Traditional medicinal plants are one of the potential sources of antimicrobial drugs and there is a great concern in the use and development of herbal medicine for the treatment of various infections. This study aimed to evaluate the antibacterial, and antioxidant activities of Dichrostachys cinera ethanolic leaves extract and to determine the components of the crude extract. D. cinera extract was evaluated against Staphylococcus aureus ATCC 25923, Escherichia coli ATCC 25922, and Pseudomonas aeruginosa ATCC 27853. The antibacterial, antioxidant activities and active constituents were determined using standard methods. Antibacterial activity of the crude extract findings showed that all bacterial candidates were susceptible where S. aureus represent MIC at 12.5 mg/ml and MBC at 25 mg/ml, E. coli and P. aeruginosa both showed MIC 25 mg/ml and MBC 50 mg/ml. In the free radical scavenging assay of the extract and the standard quercetin at concentrations of 250 μg/ml, 125 μg/ml, 50 μg/ml, 10 μg/ml, and 5 μg/ml. The radical scavenging activity for the extract was about 92%, 89.6%, 86.8%, 82.8% and 37.8% respectively, compared to quercetin which gave 89.7%, 85.8%, 62.1%, 55.5%, and 45% radical scavenging activity. The GC-Ms analysis of the total constituents demonstrated that 1,6-Anhydro-2,4-dideoxy-.beta.-D-ribo-hexo (21.26%) with different peaks, followed by Glycerin (11.56%), 1,2,3-Cyclopentanetriol (10.18%), 8,11,14-Eicosatrienoic acid, (Z,Z,Z)-(6.18%), 1H-Pyrrole, 1-methyl-(6.08%), Phytol (5.91%) and 7-Bromo-6-(2-diethylaminoethoxy)-2,3-dihyd (5.44%) as major components in the extract. Finally, this study provided useful information on the therapeutic potential of D. cinera as an antibacterial agent and recommended to be evaluated against a wide range of Bacterial and fungal strains using different solvents and different parts from the plant.

Evaluation of the Equality of Non-Polar Capillary Columns in GC/MS Analysis of Food Contact Plastics

Non-polar capillary columns for GC/MS are widely utilized in the analysis of additives for food contact materials. Though various kinds of non-polar capillary columns are commercially available, the equality of their performance has not been verified. Herein, ninety-six additives for food contact plastics were analyzed using fifteen kinds of columns, and the peak separation, retention times, and peak areas of each additive were compared. The additives, with various chemical properties, comprised forty four plasticizers, twenty lubricants, twenty antioxidants, nine ultraviolet absorbers, and three other compounds. 10 μg.mL-1 test solutions were prepared in acetone, and injected to the GC/MS. The fifteen columns were classified into five categories based on the chromatogram pattern and peak separation. To facilitate comparison of the retention time and detection sensitivity of the columns for the additives, the relative retention time (RRT) and relative peak area (RPA) were calculated by using dibutylphthalate or 4-tert-butylphenylsalicylate as an internal standard. The RRTs of the additives on each column were essentially similar. However, the RRT of the additives which were detected in the later stages differed slightly. Although the RPA of the plasticizers and lubricants were roughly similar, column-to-column differences were observed for certain additives, such as antioxidants and ultraviolet absorbers. Furthermore, certain fatty acids, antioxidants, two plasticizers, and two benzophenone type ultraviolet absorbers were not detected in the chromatograms of two columns.

LOCATION OF DOUBLE BOND POSITION OF INSECT SEX PHEROMONE BY GC/MS ANALYSIS WITH CHEMICAL IONIZATION

Ozonolysis products of four lepidopteral pheromone were identified by methane CI-MS.The spectra obtained were notably simpler than those of EI-MS,the peak of molecular ion was normally close to the base peak,and the characteristic fragment ions were high in m/z,thereby the interpretation was facilitated.

GC-MS Analysis and in Vitro Antimicrobial Susceptibility of <i>Foeniculum vulgare</i>Seed Essential Oil

Essential oil from seeds of Foeniculum vulgare was extracted on Clevenger apparatus. Essential oil was analyzed on Gas-Chromatography-Mass spectrometry (GC-MS) from which thirty six components were identified, among which 6 major and 30 minor components having different structural formulae and molecular weight representing total 99.98% of oil. Essential was investigated for its antibacterial and antifungal activity against seven infectious microbial pathogens. Paper disc diffusion and serial micro-dilution assays were performed for the determination of inhibition zone (DIZ) diameters and minimal inhibitory concentration, respectively. The Foeniculum vulgare essential oil showed the Diameter of Inhibition Zone (DIZ) ranging from 19.4 ± 0.07 - 26.4 ± 0.09 mm at a concentration level of 28 μg/disc in all the ten strains tested. The minimum inhibitory concentration (MIC) of essential oil against bacterial and fungal strains was obtained in the range of 7.0 - 56 μg/ml. Antibacterial and antifungal activity of Foeniculum vulgare essential oil is due to the presence of certain secondary plant metabolites such as terpenoids, steroids and flavonoids, esters and acids which are identified in the essential oil. The oil components can be further studied for their biological activity and overcome the problem of drug resistance in microbes.