Chemical profiling of bioactive compounds in the methanolic extract of wild leaf and callus of Vitex negundo using gas chromatographymass spectrometry

BACKGROUND The investigation of plant-based therapeutic agents in medicinal plants has revealed their presence in the extracts and provides the vision to formulate novel techniques for drug therapy.Vitex negundo(V.negundo),a perennial herb belonging to the Varbanaceae family,is extensively used in conventional medication.AIM To determine the existence of therapeutic components in leaf and callus extracts from wild V.negundo plants using gas chromatography-mass spectrometry(GCMS).METHODS In this study,we conducted GC-MS on wild plant leaf extracts and correlated the presence of constituents with those in callus extracts.Various growth regulators such as 6-benzylaminopurine(BAP),2,4-dichlorophenoxyacetic acid(2,4-D),α-naphthylacetic acid(NAA),and di-phenylurea(DPU)were added to plant leaves and in-vitro callus and grown on MS medium.RESULTS The results clearly indicated that the addition of BAP(2.0 mg/L),2,4-D(0.2 mg/mL),DPU(2.0 mg/L)and 2,4-D(0.2 mg/mL)in MS medium resulted in rapid callus development.The plant profile of Vitex extracts by GC-MS analysis showed that 24,10,and 14 bioactive constituents were detected in the methanolic extract of leaf,green callus and the methanolic extract of white loose callus,respectively.CONCLUSION Octadecadienoic acid,hexadecanoic acid and methyl ester were the major constituents in the leaf and callus methanolic extract.Octadecadienoic acid was the most common constituent in all samples.The maximum concentration of octadecadienoic acid in leaves,green callus and white loose callus was 21.93%,47.79%and 40.38%,respectively.These findings demonstrate that the concentration of octadecadienoic acid doubles in-vitro compared to in-vivo.In addition to octadecadienoic acid;butyric acid,benzene,1-methoxy-4-(1-propenyl),dospan,tridecanedialdehyde,methylcyclohexenylbutanol,chlorpyrifos,n-secondary terpene diester,anflunine and other important active compounds were also detected.All these components were only available in callus formed in-vitro.This study showed that the callus contained additional botanical characteristics compared with wild plants.Due to the presence of numerous bioactive compounds,the medical use of Vitex for various diseases has been accepted and the plant is considered an important source of therapeutics for research and development.

Comparison of simultaneous distillation extraction and solid-phase micro-extraction for determination of volatile constituents in tobacco flavor

The volatile and semi-volatile components in tobacco flavor additives were extracted by both simultaneous distillation extraction and solid-phase micro-extraction. Extraction conditions for solid-phase micro-extraction were optimized with information theory. Then, detection were accomplished by gas chromatography-mass spectrometry. Characteristic of each method was compared. Qualitative analysis and quantitative analysis of 6# tobacco flavor sample were accomplished through both simultaneous distillation extraction and solid-phase micro-extraction. The experimental results show that solid-phase micro-extraction method is the first choice for qualitative analysis and simultaneous distillation extraction is another good selection for quantitative analysis. By means of simultaneous distillation extraction, 20 components are identified, accounting for 92.77% of the total peak areas. Through solid-phase micro-extraction, there are 17 components identified accounting for 91.49% of the total peak areas. The main aromatic components in 6# tobacco flavor sample are propanoic acid, 2-hydroxy-, ethyl ester, menthol and menthyl acetate. The presented method has been successfully used for quality control of tobacco flavor.

Volatile components of Rhizoma Alpiniae Officinarum using three different extraction methods combined with gas chromatography-mass spectrometry

Volatile components from Rhizoma Alpiniae Officinarum were respectively extracted by three methods including hydrodistillation, headspace solid-phase microextraction （HS-SPME） and diethyl ether extraction. A total of 40 （hydrodistillation）, 32 （HS-SPME） and 37 （diethyl ether extraction） compounds were respectively identified by gas chromatography-mass spectrometry （GC/MS） and 22 compounds were overlapped, including β-farnesene, 7-muurolene, 2,6-dimethyl-6- （4-methyl-3-pentenyl）bicyclo[3.1.1]hept-2-ene, eucalyptol and cadina-1（10）, 4-diene and so forth, varying in relative contents. HS-SPME is fast, sample saving and solvent-free and it also can achieve similar profiles as those from hydrodistillation and solvent extraction. Therefore, it can be the priority for extracting volatile components from medicinal plants.

Multiresidue Method for Determination of 67 Pesticides in Water Samples Using Solid-Phase Extraction with Centrifugation and Gas Chromatography-Mass Spectrometry

A new multi-residue method based on solid-phase extraction (SPE) with centrifugation was developed for determination and quantitation of 67 pesticides in water samples. Two SPE cartridges were tested: Chromabond C18 and Oasis HLB. Parameters that influence the extraction efficiency such as the eluent volume, the sample loading volume, the addition of organic solvent to water sample, sorbent drying and elute concentration were optimized. The innovation of this work was the examination of the use of a centrifugation technique in both the drying and elution steps. When combined with centrifugation, the volume of the elution solvent was reduced to 2 mL and the time for sorbent drying decreased also to 10 min under vacuum. Under the optimized conditions, this method showed good recoveries higher than 65% - 68% for the 67 analyzed pesticides using the C18 and HLB cartridges with relative standard deviations lower than 9.7% - 12.3%. Limits of quantification were between 2 and 20 ng.L–1. The simplicity of the described method, use of less of organic solvent, short procedure time, and good recoveries demonstrate the advantages of this environmentally friendly approach for routine analysis of numerous samples.

Ultrasonic Nebulization Extraction Coupled with Gas Chromatography-Mass Spectrometry for Analysis of Volatile Components in Traditional Chinese Patent Medicine

The ultrasonic nebulization extraction（UNE） was developed and applied to the extraction of volatile components from traditional Chinese patent medicine Xiaoyao Pills. Several parameters of ultrasonic nebulization extraction including the sample particle size, solvent volume, extraction time and ultrasonic power were studied and selected. As a result, 2.4 g of sample with particle size of 80 mesh was extracted with 15 mL of n-hexane for 20 min at an ultrasonic power of 35 W. The volatile components were analyzed by gas chromatography-mass spectrometry （GC-MS） under the optimal conditions and 57 compounds were identified. The precision, repeatability and stability of the proposed method were also studied. Compared with ultrasonic-assisted extraction（UAE） and hydrodistillation（HD） extraction, the proposed method is more efficient, faster and easier to be operated at room temperature with smaller sample and energy consumption. It is suggested that the ultrasonic nebulization extraction can be used as a novel alternative method for the extraction of volatile components from traditional Chinese patent medicine.

Direct Determination of Polychlorinated-Biphenyls in Automotive Shredder Residues by Gas Chromatography-Mass Spectrometry

An easy and rapid method is proposed for the determination of PCBs in automotive shredder residues, using gas chromatography combined with low resolution mass spectrometry (GC-MS). It is based on direct n-hexane solid-liquid extraction, subtracting background of the lineal aliphatic hydrocarbon interferences and integration of chromatographic peaks containing selected ion PCBs masses (256, 292 and 326 m/z), which are common in all PCBs formulations. Recoveries were in the 80% - 120% range;PCBs were detected and quantified in shredder samples from an automotive shredder industry, thus indicating the validity of the method.

Response Surface Optimization of Nigella glandulifera Freyn Seed Oil Yield by Supercritical Carbon Dioxide Extraction

Supercritical carbon dioxide （SC-CO2） extraction was employed to extract oil from Nigella glandulifera Freyn seed in this study. Response surface methodology （RSM） was applied to evaluate the effects of the process parameters （pressure, temperature, and CO2 flow rate） on oil yield of N. glandulifera seed. A Box-Behnken design was used to optimize the extraction parameters. The analysis of variance indicated that the linear coefficients of pressure and CO2 flow rate, the quadratic term coefficients of pressure and temperature and the interactions between pressure and temperature, as well as temperature and CO2 flow rate, had significant effects on the oil yield （P〈0.05）. The optimal conditions to obtain the maximum oil yield from N. glandulifera seed were pressure 30.84 MPa, temperature 40.57°C, and CO2 flow rate 22.00 L h-1. Under these optimal conditions, the yield of oil was predicted to be 38.19%. The validation experiment results agreed with the predicted values. The fatty acid composition of N. glandulifera seed oil extracted using SC-CO2 was compared with that of oil obtained by Soxhlet method. The results showed that the fatty acid compositions of oil extracted by the two methods were similar. Identification of oil compounds with gas chromatography-mass spectrometry （GC-MS） showed that the contents of unsaturated fatty acids linoleic acid （48.30%）, oleic acid （22.28%） and saturated fatty acids palmitic acid （16.65%）, stearic acid （4.17%） were the most abundant fatty acids in seed oil from N. glandulifera.

Triacontyl modified silica gel as a sorbent for the preconcentration of polycyclic aromatic hydrocarbons in aqueous samples prior to gas chromatographic-mass spectrometry determination

Triacontyl modified silica gel as a sorbent coupled with gas chromatography-mass spectrometry(GC-MS) was developed to determine EPA prior 16 polycyclic aromatic hydrocarbons(PAHs) in water samples.Various parameters of solid-phase extraction such as organic modifier solvent,eluent,sample flow rate and volume were optimized.The developed method was found to yield a linear calibration curve in the concentration range of 0.05-8μg/L with respect to naphthalene,acenaphthylene,acenaphthene and 0.01-8μg/L for dibenz[a,h]anthracene and 0.05-14μg/L for fluorene,phenanthrene,anthracene and 0.01-14μg/L for the rest of analytes.Furthermore,the good accuracy and repeatability of the method made sure the requirements for achieving reliable analysis of PAHs in the environmental water samples,and the recoveries of optimal method were in the range of 80-120%except to higher volatility PAHs.C_(30)-bonded silica was proved to be an efficient sorbent for extraction of high molecular weight PAHs.

Determination of Five (5) Possible Contaminants in Recycled Cardboard Packages and Food Simulants Using Ultrasound Assisted Extraction Coupled to GC-MS

A modified analytical procedure has been developed to test for 5 organic pollutants [benzophenone, 2 diisopropylnaphthalenes (DIPNs) {2,6- and 2,7-diisopropylnapthalene} and 2 hydrogenated terphenyls (HTPs) {m-terphenyl and o-terphenyl}] that can be found as residues in recycled cardboards intended for use as food packaging materials and to test for migration levels of these compounds in a food simulant (Tenax). A main objective was to develop a modified rapid and reliable method for the identification and quantification of these compounds at low concentrations. The method was based on ultrasound-assisted solvent extraction (UAE) followed by gas chromatography-mass spectrometry (GC-MS) analysis. The developed method was applied to analyze 3 commercially available recycled carton board food-packaging materials and also to study the potential migration of the 5 organic pollutants from these materials into Tenax to check if these recycled cardboards can be considered as suitable for use in direct contact with foodstuffs. The limits of detection (LODs) of standard solutions of the 5 compounds were determined at a signal-to-noise ratio of 3. The LODs and the limits of quantification (LOQs) of examined pollutants ranged between 0.005 to 0.5 mg/kg, and 0.1 to 1 mg/kg, respectively. The extremely low amounts of most contaminants that migrate from packaging materials to Tenax indicate that the recycled cardboards tested can be safely used for direct food contact applications.

A new method of simultaneous determination of atmospheric amines in gaseous and particulate phases by gas chromatography-mass spectrometry

As more attention is being paid to the characteristics of atmospheric amines,there is also an increasing demand for reliable detection technologies.Herein,a method was developed for simultaneous detection of atmospheric amines in both gaseous and particulate phases using gas chromatography-mass spectrometry(GC-MS).The amine samples were collected with and without phosphoric acid filters,followed by derivatization with benzenesulfonyl chloride under alkaline condition prior to GC-MS analysis.Furthermore,the method was optimized and validated for determining 14 standard amines.The detection limits ranged from0.0408-0.421μg/mL(for gaseous samples)and 0.163-1.69μg/mL(for particulate samples),respectively.The obtained recoveries ranged from 68.8%-180%and the relative standard deviation was less than 30%,indicating high precision and good reliability of the method.Seven amines were simultaneously detected in gaseous and particulate samples in an industrial park using the developed method successfully.Methylamine,dimethylamine and diethylamine together accounted for 76.7%and 75.6%of particulate and gaseous samples,respectively.By comparing the measured and predicted values of gas-particle partition fractions,it was found that absorption process of aqueous phase played a more important role in the gas-partition of amines than physical adsorption.Moreover,the reaction between unprotonated amines and acid(aq.)in water phase likely promoted water absorption.Higher measured partition fraction of dibutylamine was likely due to the reaction with gaseous HCl.The developed method would help provide a deeper understanding of gas-particle partitioning as well as atmospheric evolution of amines.

同时蒸馏萃取结合GC-MS分析南北地区高粱蒸煮香气成分

为探究南北地区高粱的蒸煮香气成分和特征风味物质,该研究利用同时蒸馏萃取(SDE)结合气相色谱-质谱技术(GC-MS)分别对南北两个地区4种高粱(G1、YN4、G8、G10)的蒸煮香气及其特征风味物质进行分析,并结合香气活度值(OAV),分析南北地区高粱具有的特征风味物质。结果表明,南北地区4种高粱共检测出205种香气成分,其中南方地区两种高粱(G1、YN4)共检出147种、北方地区高粱(G8、G10)检出121种,南方地区高粱蒸煮香气成分种类较北方高粱更加丰富;北方地区高粱共有的挥发性风味物质有4种,其中4-甲基苯酚被认为是北方地区高粱的特征风味物质(OAV>1),南方地区高粱共有的挥发性风味物质有7种,其中4-乙基愈创木酚、正己酸乙酯、壬醛被认为是南方地区高粱的特征风味物质(OAV>1)。综合来看,南方高粱(G1、YN4)在特征风味物质以及香气成分种类和含量上与白酒酿造所需风味物质更加相符。

合欢树不同部位挥发油成分及其气相色谱-四极杆飞行时间串联质谱分析

目的:分析合欢树不同药用部位(合欢花、合欢米及合欢皮)中的挥发性成分及其相对含量。方法:采用同时蒸馏-萃取方法提取合欢花、合欢米及合欢皮的挥发油,并运用气相色谱-四极杆飞行时间串联质谱(GC-Q/TOF-MS)技术对其化学成分进行分析,通过NIST 14.L数据库进行化合物检索与鉴别,采用面积归一法确定各成分的相对含量。结果:从合欢花、合欢米及合欢皮挥发油中分别鉴定出主要成分80、61及42种,分别占其挥发性成分总量的96.44%、97.67%及93.36%。合欢皮的脂肪族化合物相对百分含量高于合欢米、合欢花;合欢皮的芳香族化合物、萜类化合物相对百分含量与数量明显低于合欢花和合欢米。合欢花、合欢米及合欢皮三者共有成分11种;合欢花特有成分25种,合欢米特有成分10种,合欢皮特有成分27种。结论:本研究采用GC-Q/TOF-MS技术对合欢花、合欢米及合欢皮中的挥发性成分进行比较分析,可为植物合欢的合理开发和利用提供科学依据。

Compound’s Pre-Screening of <i>Withania somnifera</i>, <i>Bacopa monnieri</i>and <i>Centella asiatica</i>Extracts

Spectral fluorescence signature, Gas Chromatography-Mass Spectrometry and Liquid Chromatography-Mass Spectrometry for identification of chemical and bioactive compounds were applied to study the plant extracts of Withania somnifera, Centella asiatica and Bacopa monnieri which are related to the possible treatment of mental diseases as Alzheimer, Parkinson and Depression. These plants are known for different positive phytotherapeutic effects on the human brain without negative post-, adverse or after effects to the treated individuals, and have been recommended in several medical studies. Therefore, we selected these plants for further analysis, based on the inhibition results of in vitro Amyloid Beta fibrillation tests made by previous measurements. With this study a first screening of the complex plant extract mixtures was performed, to get an initial overview about known and unknown ingredients. In all three plants, similar main compounds were identified, however in different quality and quantity. These may provide substantial information on which compound combinations might be mainly responsible for the positive effects and should be further investigated being responsible for reducing the fibrillation process of Amyloid Beta.

不同产地花生酱的挥发性风味成分比较分析

为研究不同提取方法比较不同产地花生酱中挥发性风味物质的差异。采用顶空固相微萃取(HS-SPME)和同时蒸馏萃取(SDE)两种方法提取4种不同国家花生酱,中国莺歌花生酱(Z)、美国四季宝花生酱(M)、澳大利亚贝科姆花生酱(A)、新西兰皮卡思花生酱(X)的挥发性风味物质,用气相色谱-质谱联用技术(GC-MS)对挥发性物质进行鉴定以内标法计算各类物质的含量,并结合气味活度值(OAV)方法分析不同风味物质对整体风味的贡献程度。结果表明:4种花生酱共鉴定出挥发性物质202种,其中SDE鉴定出70种,HS-SPME鉴定出142种。A、M、X、Z样品分别鉴定出71种、93种、58种和141种挥发性物质。HS-SPME鉴定挥发性成分更全面,而SDE法可较灵敏的检测吡嗪类和醛类成分。Z样品中含有最丰富的风味物质其中醛类风味物质含量最高为14901.17μg/kg。结合OAV分析得到:对四种花生酱的整体风味贡献程度较大的风味物质均为己醛、苯乙醛、苯乙醇、2,5-二甲基吡嗪、2-乙基-3,6-二甲基吡嗪、2-乙基-5-甲基吡嗪。Z样品的风味成分最丰富,风味品质要好于其他三种花生酱,其烤花生香味、杏味较突出。

同时蒸馏-萃取黄芪地上部分挥发油成分及其气相色谱-四极杆飞行时间串联质谱分析

目的采用同时蒸馏-萃取方法提取甘肃产黄芪地上部分挥发油,并运用气相色谱-四极杆飞行时间串联质谱(GC-Q/TOF-MS)技术对中药黄芪地上部分挥发油中的化学成分进行鉴定,为黄芪的进一步开发和利用提供理论依据。方法应用GC-Q/TOF-MS检测挥发油中的化学成分,通过NIST 14.L数据库进行化合物检索并鉴别,采用面积归一法确定各成分的相对含量。结果共鉴定出挥发性成分66种,占挥发油总量的93.62%。主要包括脂肪族化合物(79.48%),芳香族化合物(6.71%)和萜类化合物(4.68%)。脂肪族成分主要为植物醇(16.84%),1-辛烯-3-醇(15.42%),反式-3-己烯-1-醇(9.51%)。芳香族成分主要为苯甲醇(2.68%),苯乙醇(1.84%)。萜类成分主要为芳樟醇(2.98%)。结论GC-Q/TOF-MS技术能准确快速地鉴定黄芪地上部分挥发油,且挥发油化学成分丰富,为黄芪药材挥发油的进一步开发和利用提供新思路。

同时蒸馏萃取法结合气-质联用分析碰碰香精油成分

采用同时蒸馏萃取法提取碰碰香精油,通过气相色谱-质谱联用仪分析其化学成分。从碰碰香精油中鉴定出86种挥发性成分,占精油总成分的91.34%;主要特征成分为5α-雄甾烷-3,17-二酮和D-柠檬酸,其相对百分比分别为31.49%和18.58%;鉴定出43种萜烯类化合物,占精油相对百分比34.62%。为碰碰香资源充分利用与深度开发提供参考依据。

GC-MS测定煮鸭蛋中挥发性风味物质

为了研究煮鸭蛋中的挥发性风味物质,采用同时蒸馏萃取法对其进行萃取,同时对萃取条件进行了优化,之后采用气相色谱-质谱法对其挥发性风味成分进行了定性分析。结果表明,煮鸭蛋中鉴定出59种物质,即烃类11种、醇类9种、醛5种、酮3种、酸7种、酯20种、含硫及杂环物质4种,相对含量分别为23.769%、2.045%、9.624%、7.271%、7.259%、39.501%、10.531%。

不同萃取方式下熟化马铃薯挥发性物质分析

【目的】探明熟化马铃薯挥发性风味物质。【方法】分别采用同时蒸馏萃取(SDE)法和顶空固相微萃取(HS-SPME)法提取熟化马铃薯的挥发性风味物质,结合气相色谱-质谱联用(GC-MS)对其挥发性化合物进行分析。【结果】2种萃取方法共鉴定出53种挥发性风味物质,其中,SDE法鉴定出24种,醛类、醇类和杂环化合物鉴定物质占比较多,相对含量分别占挥发性风味物质总量的44.27%、23.79%和18.34%;其次是酮类、烷烃类和酯类物质,相对含量为1.00%以上;酸类物质相对含量最低,为0.83%。HS-SPME法鉴定出29种,为醛类、醇类、酮类、杂环化合物和其他物质,其中醛类物质最多,占比73.57%,烷烃类、酯类和酸类均未检出。【结论】2种萃取方法共同鉴定出的挥发性风味物质有10种,以醛类为主,被认为是熟化马铃薯的主体风味成分,其中,3-甲硫基丙醛、5-甲基呋喃醛、苯乙醛和壬醛相对含量较高,初步判定是马铃薯的关键香气成分。

基于同时蒸馏萃取-气质联用法(SDE-GC-MS)分析不同品种原料坦洋工夫红茶的香气组分

【目的】分析不同品种原料制作的传统型坦洋工夫红茶香气组分,为了解品种与香气间的相关性、提升红茶加工工艺提供参考。【方法】以‘金牡丹’‘茗科1号(金观音)’‘坦洋菜茶’‘福安大白茶’‘梅占’等不同品种一芽二、三叶鲜叶为原料,按照传统型坦洋工夫红茶初制工艺加工红茶,采用同时蒸馏萃取法(SDE)结合气相色谱-质谱联用法(GC-MS)检测其香气组分,分析不同红茶样的香气组成,并进行感官审评与相关性分析等。【结果】经SDE-GC-MS检测,5个红茶样中各类香气组分共计109种,其中金牡丹香气组分最多,高达52种;香气种类含量最高的是醇类,其次为酯类、醛类等;金观音中香叶醇相对含量为最高,达48.13%;梅占中芳樟醇及壬醛相对含量均最高,分别为22.97%、12.82%;坦洋菜茶中松油醇相对含量最高,为1.78%;3,7-二甲基-1,5,7-辛烯-3-醇在福安大白茶相对含量最高,为11.66%;参试品种均含有香叶醇或其异构体、芳樟醇等重要的香气成分。感官审评结果表明,参试品种均呈现良好的香气,其中金牡丹香气和滋味中花果香最明显,感官审评得分最高;聚类分析表明,金牡丹与坦洋菜茶、梅占与福安大白茶香气成分最为相似;相关性分析表明,香气、滋味得分与香气组分含量具有一定相关性。【结论】5个茶树品种均适制优质坦洋工夫红茶,其香气组分含量与茶树品种、加工工艺有一定关联性。品种间香气组分含量及比例的差异性,是造成不同品种原料坦洋工夫红茶香气呈现不同特征的重要原因。

凝胶渗透色谱和气相色谱-质谱法测定动物食品中27种有机氯和15种拟除虫菊酯类农药残留量

A GC-MS method for the determination of 27 organochlorine pesticides and 15 Pyrethroid pesticides in animal food is established.The method was based on Gel Permeation chromatography combined with solid-phase extraction for sample preparation.Rapid qualitative and quantitative analyses was carried out by gas chromatography-mass spectrometry under the selective-ion monitoring mode.The experimental results showed that the correlation coefficients were better than 0.99,the recoveries for spiked standards were 70%-104%,the relative standard deviations were 2.1%-15.9%.