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.

GC-MS Analysis and Antibacterial Activity Study of Volatile Oil from 11 Kinds of Aurantii Fructus Immaturus Processed Products

[Objectives]To study the volatile components and antibacterial effects of 11 kinds of Aurantii Fructus Immaturus processed products.[Methods]11 kinds of Aurantii Fructus Immaturus processed products were obtained according to the traditional processing method,the volatile oil was extracted by steam distillation,and the composition of volatile oil in the 11 kinds of processed products was analyzed by gas chromatography-mass spectrometry(GC-MS).the relative percentage content of each component in these 11 kinds of processed products was determined using the peak area normalization.The drug sensitivity activity of the volatile oil of these 11 kinds of processed products was tested using the K-B paper diffusion method and the minimum inhibition volume fraction of volatile oil of these 11 kinds of processed products was tested using the microdilution method.[Results]The highest yield of volatile oil of 11 kinds of these processed products was baking(5.193%),and the lowest was stir-bake to scorch(1.998%).A total of 36 chemical components were identified from the volatile oils of these 11 kinds of processed products.The components with the most volatile oil were stir-bake to scorch(24 kinds),and the components with the least volatile oil were the method of processing with rice-washed water(15 kinds).They contain 8 kinds of common chemical components,such as limonene,linalool,myrcene,α-pinene.The highest content of limonene came from processing with honey(60.93%),the lowest came from processing with rice-washed water(55.25%);the highest content of linalool came from processing with rice-washed water(7.139%),the lowest came from processing with honey(5.436%);the highest content of myrcene came from processing with honey(1.899%),the lowest came from stir-bake to scorch(1.632%);the highest content ofα-pinene came from raw Aurantii Fructus Immaturus(2.355%),and the lowest came from stir-bake to scorch(1.618%).The volatile oil of these 11 kinds of Aurantii Fructus Immaturus processed products has good antibacterial effect on Escherichia coli and Staphylococcus aureus.[Conclusions]The oil yields of volatile oils of 11 kinds of Aurantii Fructus Immaturus processed products are different,the content of limonene is significantly different,and the changes of other chemical components and their contents are not significantly different.The volatile oil of 11 kinds of Aurantii Fructus Immaturus processed products has certain antibacterial effect.

Analysis of the Volatile Components of Polygonum chinense L.Extracted with Different Solvents by GC-MS

[Objectives]This study was conducted to investigate the volatile components of Polygonum chinense L.[Methods]The volatile components of the methanol extract,ethyl acetate extract,chloroform extract and petroleum ether extract of P.chinense were analyzed and determined by gas chromatography.[Results]The volatile components of the methanol extract from P.chinense were the most,and phenolic acids and ketones accounted for a relatively high proportion,among which pyrogallic acid had the highest content.The ethyl acetate extract contained the second most volatile components,mostly acids and esters,of whichβ-sitosterol had the highest content;the chloroform and petroleum ether extracts had relatively few types of volatile components,most of which were alkanes,and the content ofγ-sitosterol shared by the two was the highest.The common substances of the four extracts were palmitic acid and phytol.[Conclusions]This study provides a theoretical basis for the quality evaluation of P.chinense and a scientific basis for its resource development.

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.

蒙山名茶蒙顶甘露和蒙山毛峰特征香气成分的GC-MS测定与分析

采用同时蒸馏萃取法和气相色谱质谱（gas chromatography-mass spectrometry ， GC-MS）分析方法系统分析了蒙山茶原产地保护区域内蒙泉、后盐、陇西3个产地及保护区外合江产地蒙顶甘露和蒙山毛峰香气成分的特征与差异.结果表明，在鉴定的63种香气成分中，醇类和醛类占一半以上（59.16％～71.42％）.在蒙顶甘露和蒙山毛峰的香气组分中均以植醇、香叶醇、L-芳樟醇、壬醛和正庚醛这5个成分所占比例较高；保护区内蒙顶甘露和蒙山毛峰最重要的香气特征是植醇和壬醛含量显著高于保护区外，其总量分别占保护区中心内甘露的29.95％和毛峰的40％、保护区外甘露的0％和毛峰的11.27％，同时也是区别于其他名优绿茶的最主要的香气成分.由保护区中心向外延伸，蒙顶甘露和蒙山毛峰的香型有相似的变化规律：由保护区中心的板栗香型经中间的铃兰类鲜爽花香型逐渐过渡至边沿的蜜糖香、花香型.总体上，原产地保护区域内蒙顶甘露和蒙山毛峰的香气品质优于其他非原产地保护区域的蒙顶甘露和蒙山毛峰.

广西八角挥发油的提取研究与GC-MS分析

In this paper,the Illilium verum Hook.f.grow at mountain of Dayao of Jinxiu in Guangxi,Volatile oil was extracted by soxhet method and steam distillation.All the volatile oil was analyzed by GC-MS,the result show the ingredients and rate of product were change greatly,The major chemical constituents were trans-anethole,estragole and anisaldehyde etc.

藏药甘肃蚤缀脂溶性成分的GC-MS分析

研究藏药甘肃蚤缀的脂溶性成分,进一步揭示该药材的化学成分,为这一传统藏药资源的开发利用提供实验依据。采用95%乙醇回流提取甘肃蚤缀全草,滤液浓缩后用石油醚萃取,得到脂溶性部位,通过气相色谱-质谱联用技术分析其化学成分,结合计算机检索技术及美国国家标准技术研究所(NIST)化合物谱库检索进行鉴定,采用面积归一化法确定其相对含量。从甘肃蚤缀石油醚部位共分离鉴定出25个化合物,相对含量占总含量的91.31%,包括脂肪类、甾体、三萜及芳香化合物等。

基于GC-FID、HS-SPME-GC-MS与电子鼻技术评价不同水果发酵酒的香气特征

采用气相色谱-氢火焰离子化检测器法(gas chromatography with hydrogen flame ionization detection,GCFID)、顶空固相微萃取-气相色谱-质谱(headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry,HS-SPME-GC-MS)和电子鼻技术分析6种果酒中的挥发性成分,评价果酒风味轮廓特征的差异性。结果表明,GC-FID定量测定樱桃李酒,其中异戊醇、活性戊醇、β-苯乙醇含量最高,乙酸乙酯含量最低;木瓜酒中正丙醇、2,3-丁二醇、癸酸乙酯、乙酸含量最高; 3-羟基-2-丁酮含量在樱桃李酒中最高,山楂酒、甜橙酒中最少。HP-SPME-GC-MS鉴定果酒中挥发性物质94种,其中醇类23种,酯类43种,醛酮类10种,酸类8种,酚类2种,苯环类5种,烷烃类3种。山楂酒、菠萝酒、木瓜酒、甜橙酒、无花果酒和樱桃李酒中香气物质数量分别为34、44、45、45、33、47种。其中山楂酒、木瓜酒和无花果酒中未检出酚类、烷烃类物质。电子鼻对不同果酒香气的区分效果无重叠,W5S传感器区分果酒香气能力最强。比较而言,菠萝酒和樱桃李酒的口感更圆润,香气更愉悦,感官得分最高。

Rapid on-site identification of hazardous organic compounds at fire scenes using person-portable gas chromatography-mass spectrometry(GC-MS)—part 1:air sampling and analysis

Recent advancements in person-portable instrumentation have resulted in the potential to provide contemporaneous results through rapid in-field analyses.These technologies can be utilised in emergency response scenarios to aid first responders in appropriate site risk assessment and management.Large metropolitan fires can pose great risk to human and environmental health due to the rapid release of hazardous compounds into the atmosphere.Understanding the release of these hazardous organics is critical in understanding their associated risks.Person-portable gas chromatography-mass spectrometry(GC-MS)was evaluated for its potential to provide rapid on-site analysis for real-time monitoring of hazardous organic compounds at fire scenes.Air sampling and analysis methods were developed for scenes of this nature.Controlled field testing demonstrated that the portable GC-MS was able to provide preliminary analytical results on the volatile organic compounds present in air samples collected from both active and extinguished fires.In-field results were confirmed using conventional laboratory-based air sampling and analysis procedures.The deployment of portable instrumentation could provide first responders with a rapid on-site assessment tool for the appropriate management of scenes,thereby ensuring environmental and human health is proactively protected and scientifically informed decisions are made for the provision of timely advice to stakeholders.

福建姜黄挥发油化学成分的HS-SPME-GC-MS分析

采用水蒸气蒸馏法提取福建姜黄挥发油,应用顶空固相微萃取进样结合气相色谱-串联质谱联用技术(HS-SPME-GC-MS)分析姜黄挥发油的化学成分。结果表明:姜黄挥发油含有量为7.2%(mL/g),从姜黄挥发油中共分出62个色谱峰,初步鉴定出了其中的51种化学成分,占总挥发油总量的98.41%。在鉴定的化合物中,主要为单萜类化合物和倍半萜类化合物,其中新发现一种主要成分为β-柏木烯,相对含量占比高达26.58%,这可作为福建姜黄挥发油的特征成分和主要品质指标。本研究结果将为福建姜黄植物药材的品质评价提供科学依据。

GC-MS法测定黄酒和食用酒精中的氨基甲酸乙酯

建立应用气相色谱-质谱联用法(gas chromatography-mass spectrometry,GC-MS)快速测定黄酒和食用酒精中氨基甲酸乙酯(ethylcarbamate,EC)的分析方法。以黄酒和食用酒精为研究对象,样品经过碱性硅藻土固相萃取柱净化、浓缩后,用GC-MS进行测定,同位素内标法定量。氨基甲酸乙酯在10~600μg/L线性关系良好,相关系数r^2=0.999 3。加标水平为5、100、250μg/kg 3个浓度条件下,在黄酒中的加标回收率为81.2%~89.5%,每个加标水平测定6次的相对标准偏差(RSD)为3.7%~5.0%;在食用酒精中的加标回收率为91.2%~99.4%,每个加标水平测定6次的RSD为3.1%~4.1%。方法的检出限为1.0μg/kg,方法的定量限为3.0μg/kg。该方法定量准确、操作简便、灵敏度高,适用于黄酒和食用酒精中氨基甲酸乙酯的测定。

Determination of Aromatic Components of Rosa davurica Pall. by Headspace Solid Phase Microextraction Combined with GC-MS

[Objectives] To determine the aromatic components of Rosa davurica Pall. [Methods] 42 kinds of aromatic components were identified from the flowers of R. davurica by headspace solid phase microextraction( HS-SPME) combined with gas chromatography-mass spectrometry( GC-MS). The main compounds were alcohols( 54. 88%) and aldehydes( 19. 55%). [Results] The top five components with the highest relative content were phenylethyl alcohol( 12. 69%),geraniol( 9. 85%),citronellol( 8. 80%),nerol( 7. 84%) and 2-n-pentylfuran( 7. 45%). [Conclusions] Headspace solid phase microextraction( HS-SPME) combined with gas chromatography-mass spectrometry( GC-MS) can provide basis for further development and utilization of R. davurica.

Transcriptome analysis of the influence of CPPU application for fruit setting on melon volatile content

In fruit production,the application of the plant growth regulator 1-(2-chloro-4-pyridyl)-3-phenylurea(CPPU)dulls the fruit aroma.Gas chromatography-mass spectrometry and transcriptome analyses were performed on CPPU-treated and pollinated fruits to determine how CPPU affects the production of aroma in melon fruit.The results showed that the contents of two important esters(benzyl acetate and phenethyl acetate)in the CPPU-treated fruits were significantly lower than those in the pollinated fruits.Transcriptome sequencing data revealed that most differentially expressed genes were involved in“phenylalanine metabolism”pathway,and their expression was significantly decreased in the CPPU-treated fruits.Further analysis showed that the phenylalanine content in the CPPU-treated fruits was significantly higher than that in the pollinated fruits.In summary,CPPU application interferes with phenylalanine metabolism in melon fruits and affects the production of aromatic esters.

Studies on the Components of Essential Oil of <i>Zanthoxylum Armatum</i>by Gc-Ms

The essential oil of Zanthoxylum armatum was extracted through hydro distillation and analyzed by GC-MS. Hydrocarbon fraction (17.35%) of the oil was much lower and oxygenated compounds comprised fairly high portion of essential oil (39.21%). Percentages of monoterpenes and sesquiterpenes found were 47.33% and 10.83% respectively. Oxygenated monoterpenes comprised major profile of chromatogram of essential oil of Zanthoxylum armatum i.e. 37.23% where as monoterpene hydrocarbons were 10.09%. Alcoholic percentage was much higher i.e. 26.76% and 15-hexadecanoloide (6.58%) the only cyclic ester was found in relatively high percentage.

The analysis of volatile flavor components of Jin Xiang garlic and Tai’an garlic

The volatile flavor compounds of Jin Xiang garlic and Tai’an garlic in chemical composition were detected and analyzed and the contents of them were compared and determinated. The volatile constituents of Jin Xiang garlic and Tai’an garlic were compared and analyzed by automatic static headspace and gas chromatography-mass spectrometry. Qualitative analysis of samples was made through the analysis of gas chromatography-mass spectrometry and NIST mass spectral library computer retrieval, and quantitative analysis was made by using area normalization method. The analysis results show that the slight difference of the volatile flavor compounds was detected in different places of origin garlic and Jin Xiang garlic was detected more total sulfur-containing compounds than Tai’an garlic. Meanwhile, the contents of sulfur compounds of the fresh garlic were more than the stored garlic and there were significant differences between them. The tests results indicated that flavor substances’ types were slightly different between Jin Xiang garlic and Tai’an garlic, and regional differences cannot affect the garlic flavor substances type. Jin Xiang garlic has more obvious flavor substances than Tai’an garlic which play a decisive role in the garlic flavor, such as 1,3-dithiane, and allyl trisulfide and allyl disulfide and diallyl tetrasulphide. The result of this research indicates that Automatic static headspace and gas chromatography-mass spectrometry is a fast, easy, efficient and accurate method to analyze and identify the volatile flavor components of garlic.

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.

Application of Mass Spectrometry (MS)-coupled Techniques in Pesticide Residue Detection

Pesticide residue detection is an important work to ensure the quality safety of agricultural products.In the process of agricultural production,in order to prevent and control agricultural diseases and pests,a certain amount of pesticides need to be used.However,if pesticides are used excessively,there will be certain pesticide residues in crops and related products.Therefore,it is necessary to do a good job in pesticide residue detection.The gas chromatography-mass spectrometry(GC-MS)and liquid chromatography-mass spectrometry(LC-MS)detection methods have good results and can effectively detect pesticide residues in related products.This paper reviewed and analyzed the application of GC-MS and LC-MS in pesticide residue detection,and proposed optimization measures based on practical experience,hoping to provide reference for relevant scholars.

Modern approaches for detection of volatile organic compounds in metabolic studies focusing on pathogenic bacteria:Current state of the art

Pathogenic microorganisms produce numerous metabolites,including volatile organic compounds(VOCs).Monitoring these metabolites in biological matrices(e.g.,urine,blood,or breath)can reveal the presence of specific microorganisms,enabling the early diagnosis of infections and the timely implementation of tar-geted therapy.However,complex matrices only contain trace levels of VOCs,and their constituent com-ponents can hinder determination of these compounds.Therefore,modern analytical techniques enabling the non-invasive identification and precise quantification of microbial VOCs are needed.In this paper,we discuss bacterial VOC analysis under in vitro conditions,in animal models and disease diagnosis in humans,including techniques for offline and online analysis in clinical settings.We also consider the advantages and limitations of novel microextraction techniques used to prepare biological samples for VOC analysis,in addition to reviewing current clinical studies on bacterial volatilomes that address inter-species in-teractions,the kinetics of VOC metabolism,and species-and drug-resistance specificity.

Exploring Chemovar-Specific Cannabis Extracts Quantification and Evaluation of Cytotoxic Compounds for Targeting Glioblastoma Multiforme

Glioblastoma Multiforme (GBM) represents one of the most aggressive and metastatic brain tumors, with a dismal success rate of less than three percent after five years, particularly in tumors with active immune checkpoints. This necessitates the development of targeted endogenous agents for precise GBM treatment. Previous experiments utilizing Chemovar Specific Cannabis Extractions (CSCEs), fractionated with polar solvents and quantified using Liquid and Gas Column Chromatography combined with Mass Spectrometry (LC/GCMS), have shown reduced viability and motility in human GBM cell lines. However, the complexity of the botanical substance has hindered the personalization of standard cannabis medicines for GBM due to unknown synergistic effects of multiple compounds. To address this limitation, our study focuses on exposing AM251 cells to chemovar fractions extracted using a non-polar solvent, thereby isolating a broader spectrum of constituents. By employing LC/GCMS in conjunction with Nuclear Magnetic Resonance (NMR), we have identified and quantified nine* compounds present in the non-polar CSCE that exhibit significant efficacy (0.1 μM) in inducing cytotoxicity* in GBM tumor cells. Conversely, the polar fraction in our experiment did not demonstrate efficacy against UM251 cells. The quantification of individual compounds within a cannabis extraction that selectively induces cell death in brain tumors holds promise for guiding future research and facilitating the development of a standardized CSCE for GBM therapy.

Determination of Chlorpyrifos in Human Blood by Gas Chromatography-Mass Spectrometry

Gas chromatography-mass spectrometry method was developed for the qualitative and quantitative analyses of chlorpyrifos in human blood samples.The chlorpyrifos and parathion(internal standard)in human blood were extracted with a mixed solvent of hexane and acetonitrile.Chlorpyrifos was well separated from the internal standard.The linear range of chlorpyrifos was 0.01-2 μg/ml in blood.The limit of detection and limit of quantification were estimated at 0.002 and 0.01μg/ml,respectively.The inter-and intra-day precisions,accuracy,and recovery were assessed to verify this method.The results showed that the developed method is rapid,sensitive,and reliable.It is suitable for the determination of chlorpyrifos in forensic toxicological analysis and clinical diagnosis.