Extraction of essential oil from shaddock peel and analysis of its components by gas chromatography-mass spectrometry

Essential oil, with more than thirty kinds of compounds separated and identified by gas chromatography-mass spectrometry, was extracted from Shatian shaddock peel and Sweet shaddock peel by squeeze-steam distillation and direct steam distillation method. Among their composition, the main components are terpene compounds, which account for 93.926% (mass fraction, the same below) and 85.843% of essential oils extracted from Shatian shaddock peel and Sweet shaddock peel, respectively. Although nootkatone is the major contributor of shaddock characteristic scent, and its contents are 1.069% and 1.749% of essential oils from Sweet shaddock peel and Shatian shaddock peel, respectively. The results show that squeeze-steam distillation gives higher yield and good quality of essential oil and the compositions of essential oils from two kinds of shaddock peels are different, but the main contributors of the shaddock scent are the same.

Headspace Solid-Phase Micro-Extraction Gas Chromatography/Mass Spectrometry(HS-SPME-GC/MS)-Based Untargeted Metabolomics Analysis for Comparing the Volatile Components from 12 Panax Herbal Medicines

Quality control of ginseng currently is mainly based on ginsenoside analysis,but rarely focuses on the volatile organic components.In the current work,an untargeted metabolomics approach,by headspace solid-phase micro-extraction gas chromatography/mass spectrometry(HS-SPME-GC/MS),was elaborated and further employed to holistically compare the compositional difference of the volatile components simultaneously from 12 Panax herbal medicines,which included P.ginseng(PG),P.quinquefolius(PQ),P.notoginseng(PN),red ginseng(PGR),P.ginseng leaf(PGL),P.quinquefolius leaf(PQL),P.notoginseng leaf(PNL),P.ginseng flower(PGF),P.quinquefolius flower(PQF),P.notoginseng flower(PNF),P.japonicus(PJ),and P.japonicus var.major(PJvm).Chromatographic separation was performed on an HP-5MS elastic quartz capillary column using helium as the carrier gas,enabling good resolution within 1 h.We were able to characterize totally 259 volatile compounds,including 82 terpenes(T),46 alcohols(Alc),29 ketones(K),25 aldehydes(Ald),21 esters(E),and the others.By analyzing 90 batches of ginseng samples based on the untargeted metabolomics workflows,236 differential ions were unveiled,and accordingly 36 differential volatile components were discovered.It is the first report that simultaneously compares the compositional difference of volatile components among 12 Panax herbal medicines,and useful information is provided for the quality control of ginseng aside from the well-known ginsenosides.

ANALYSIS OF VOLATILE CONSTITUENTS OF CHINESE MEDICINAL HERBS BY FLASH DISTILLATION/CAPILLARY GAS CHROMATOGRAPHY/MASS SPECTROMETRY

In present work,the volatile constituents of Curcuma longa L.,A.lancea (Thunb.) DC.,Foeniculum vulgare Mill,and Cinnamomun cassia Presl.have been analyzed by flash distillation/capillary gas chro-matography/mass spectrometry.The results are consistent with those obtained by conventional steam distillation extraction method.The optimum condition of flash distillation has been studied.The experimental results showed that this new technique proved to be a simple,rapid and efficient tool for microanalysis of volatile constituents of Chinese medicinal herbs.

Chemical component analysis of volatile oil in drug pair Herba Ephedrae-Ramulus Cinnamomi by GC-MS and CRM

Active volatile components in drug pair(DP)Herba Ephedrae-Ramulus Cinnamomi(HE-RC),single drug HE and RC were analyzed by gas chromatography/mass spectrometry(GC/MS),chemometric resolution method(CRM)and overall volume integration.By means of CRM,the two-dimensional data obtained from GC-MS instruments were resolved into a pure chromatogram and a mass spectrum of each chemical compound.In total,97,62,and 78 volatile chemical components in volatile oil of HE,RC,and DP HE-RC,were respectively determined qualitatively and quantitatively,accounting for 90.08%,91.62%,and 89.76% total contents of volatile oil of HE,RC,and DP HE-RC respectively.It is further demonstrated that the numbers of volatile components of DP HE-RC are almost the sum of those of two single drugs,but some relative contents of them are changed.Some new components,such as 1,6-dimethylhepta-1,3,5-triene,tetracyclo[4.2.1.1(2,5).0(9,10)]deca-3,7-diene,globulol and(E,E)-6,10,14-trimethyl-5,9,13-pentadecatrien-2-one are found in DP HE-RC because of chemical reactions and physical changes during decoction.

GC-MS Analysis of Volatile Oils in Mango Leaves from Different Producing Areas

[Objectives]To analyze the composition of volatile oils from mango leaves from different producing areas.[Methods]The volatile oils in mango leaves from different areas was extracted by steam distillation,and the GC-MS method combined with retention index and peak area normalization method was used for qualitative and quantitative analysis.[Results]The volatile oils of mango leaves in southern provinces contained high content of terpenes,such asα-gurjunene(18.39%-34.13%),(+)-viridiflorene(8.95%-16.30%)and(E)-β-ocimene(3.49%-7.63%).The volatile oils components of mango leaves were significantly different in different provinces,for example,mango leaves produced in Hainan Province contained a large amount ofβ-selinene(23.00%),but not in other provinces.[Conclusions]The origin had a great influence on the composition and contents of volatile oils in mango leaves.

Mechanism of volatile oil from Chuanxiong(Chuanxiong Rhizoma)-Suhexiang(Styrax)-Bingpian(Borneolum)in treating angina pectoris based on network pharmacology and its protective effects on myocardial damage in rats

Objective To explore the pharmacodynamic material basis and mechanism of action of volatile oil from Chuanxiong(Chuanxiong Rhizoma)-Suhexiang(Styrax)-Bingpian(Borneolum)(hereinafter referred to as C-S-B volatile oil)in treating angina pectoris based on network pharmacology and to detect its protective effects against rat myocardial damage.Methods Gas chromatography-mass spectrometry(GC-MS)was used to determine the constituents of volatile oils from Chuanxiong(Chuanxiong Rhizoma),Suhexiang(Styrax),and Bingpian(Borneolum),and the targets of the three main constituents were found predicted and screened using the PharmMapper server,and Gene Cards and Coo LGe N databases.The STRING database and Cytoscape software were used to draw the protein-protein interaction(PPI)network,RStudio software was used to analyze Gene Ontology(GO)and Kyoto Encyclopedia of Genome and Genome(KEGG)pathways,and Cytoscape software was used to construct the component-target-pathwaydisease network.The rat model of myocardial injury was established by intraperitoneal injection of a large dose of isoprenaline hydrochloride.After continuous intervention with C-S-B volatile oil for 14 d,the ejection fraction(EF)and short axis shortening rate(FS)of the left ventricle were detected.The indices of myocardial damage were detected after hematoxylin-eosin(HE)staining.Results Fifteen volatile oil components from the C-S-B formula were identified.There are 470 targets of these volatile oil components and 401 angina-related genes.There are 28 core targets,including CHRM4,ADRA1 A,FGFR1,CHRM2,CYP2 A6,CHRM5,CHRM1,CHRM3,HDAC2,and MPO,etc..The results of the KEGG analysis indicated that the C-S-B formula probably interferes with the following pathways:neuroactive ligand-receptor interactions,calcium signaling,cytochrome P450 metabolism of heteropoietin,among others.The results of animal experiments showed that the C-S-B formula essential oil could significantly improve the following myocardial indices in rats with myocardial injury:EF,FS,left ventricular end-systolic diameter(LVIDs),left ventricular end-diastolic diameter(LVIDd),and stroke volume(SV),and all the differences were statistically significant(P<0.01).Conclusion The mechanism of action of volatile oil components in the C-S-B formula in treating angina pectoris was analyzed using multi-component,multi-target and multi-pathway systems,which has laid a foundation for further revealing its mechanism of action.Animal experiments have shown that the volatile oil of the C-S-B formula can improve EF,FS,and other indices of myocardial damage in a rat model,thus relieving myocardial damage caused by heart hyperactivity,improving cardiac function,and protecting against myocardial damage.

Study on the Specific GC Chromatograms of Volatile Oil from Xinyi Biyan Pills

[Objectives]This study was conducted to establish characteristic chromatograms of of the volatile oil of Xinyi Biyan Pills by gas chromatography,discover possible problems in the production processes of different manufacturers,and further improve the quality control methods.[Methods]The volatile oil in samples was extracted and tested by gas chromatography to collect chromatograms,which were analyze and evaluated by the similarity evaluation software of chromatographic fingerprints of traditional Chinese medicine.[Results]Nineteen common peaks were calibrated in the characteristic chromatograms;and the characteristic chromatograms of samples produced by different manufacturers were obviously different.[Conclusions]Controlling the volatile components in Xinyi Biyan Pills by the established characteristic chromatograms of GC is accurate and feasible,and can be used as a quality control method for Xinyi Biyan Pills.

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.

An improved oil recovery prediction method for volatile oil reservoirs

To describe the complex phase transformation in the process of depletion exploitation of volatile oil reservoir,four fluid phases are defined,and production and remaining volume of these phases are calculated based on the principle of surface volume balance,then the recovery prediction method of volatile oil reservoir considering the influence of condensate content in released solution gas and the correction method of multiple degassing experiments data are established.Taking three typical kinds of crude oil(black oil,medium-weak volatile oil,strong volatile oil)as examples,the new improved method is used to simulate constant volume depletion experiments based on the corrected data of multiple degassing experiment to verify the reliability of the modified method.By using"experimental data and traditional method","corrected data and traditional method"and"corrected data and modified method",recovery factors of these three typical kinds of oil are calculated respectively.The source of parameters and the calculation methods have little effect on the recovery of typical black oil.However,with the increase of crude oil volatility,the oil recovery will be seriously underestimated by using experimental data or traditional method.The combination of"corrected data and modified method"considers the influence of condensate in gas phase in both experimental parameters and calculation method,and has good applicability to typical black oil and volatile oil.The strong shrinkage of volatile oil makes more"liquid oil"convert to"gaseous oil",so volatile oil reservoir can reach very high oil recovery by depletion drive.

Gas chromatography-mass spectrometry analysis of essential oils from five parts of Chaihu(Radix Bupleuri Chinensis)

OBJECTIVE: To analyze the essential oils from flowers, leaves, stems, roots, and fruits of Chaihu(Radix Bupleuri Chinensis).METHODS: We extracted essential oils from different parts of Chaihu(Radix Bupleuri Chinensis) using a steam distillation method. The essential oils were analyzed by gas chromatography-mass spectrometry(GC-MS). Data were collected in full scan mode(m/z 60-600). Volatile components were identified based on their retention indices and by comparing their mass spectra with those in the National Institute of Standards and Technology 2005 database assisted by tandem mass spectrometry information. The relative content of each constituent wasdetermined by area normalization.RESULTS: We identified 111 components, of which12 were common to all 5 parts, 30 were found only in roots, 14 were found only in flowers, 6 were found only in leaves, 4 were found only in stems,and 17 were found only in fruits.CONCLUSION: Our results show that the stems,flowers, leaves, and fruits of Chaihu(Radix Bupleuri Chinensis)contain a high concentration of essential oils, and that the exact composition of the essential oils differs among the plant parts. To develop new medicines and make full use of the Chaihu(Radix Bupleuri Chinensis)resource, it is important to characterize the essential oils from different parts of the plant. In future research, it will be important to determine the pharmacological effects of the various components and the essential oil mixtures.

Gas Chromatography–Mass Spectrometry for Quantitative and Qualitative Analysis of Essential Oil from Curcuma wenyujin Rhizomes

Objectives:A rapid and sensitive gas chromatography–mass spectrometry(GC–MS)method for quantitative and qualitative analysis of essential oil from Curcuma wenyujin rhizomes was established.Methods:The essential oil of C.wenyujin rhizomes was extracted by supercritical CO2 extraction(SFE).Six main bioactive compounds(eucalyptol,β-elemene,curzerene,germacrone,curdione,and curcumol)were analyzed in selected ion monitoring mode(SIM).Results:Curzerene is not originally present in C.wenyujin rhizomes,but is a product of the transformation of furanodiene at high temperature.The six target components demonstrated good linearity(R2>0.9979)over a relatively wide concentration range.The interday and intraday variations had relative standard deviation values less than 5%and the average recovery ranged from 96.95%to 100.04%.The limit of quantitation ranged from 0.032 to 0.235μg/mL.The developed method was successfully used to analyze the six compounds in 17 samples collected from different origins.Significant variation was observed for the concentrations of the six compounds.In addition,51 constituents were identified in C.wenyujin rhizome essential oil,consisting of 87.66%of the total essential oil,including curdione,curzerene,dehydrocurdione,germacrone,1,4-bis(2-benzimidazoyl)benzene,neocurdione,curcumenone,andβ-elemene.Conclusions:The proposed method will be useful in the quality control of C.wenyujin rhizome essential oil production.

Off－line Two－Dimensional Gas Chromatography－Mass Spectrometry for Analysis of Essential Oil of Medicinal Herb──Use of Absorption Trap

he use of an absorption trap off-line two-dimensional gas chromatography (2-DGC) in conjunction with a mass spectrometer greatly improved the separation andidefitification of minor constituents of a complex mixture such as a natural essentialoil. The absorption trap device used as an interface of 2-DGC offered the advantageof convenient manipulation.

Qualitative Analysis of A Sulfur-fumigated Chinese Herbal Medicine by Comprehensive Two-Dimensional Gas Chromatography and High-Resolution Time of Flight MassSpectrometry Using Colorized Fuzzy Difference Data Processing

To investigate the chemical transformation of volatile compounds in sulfur-fumigated Radix Angelicae Sinensis. A comprehensive two-dimensional gas chromatography (GCxGC) and high-resolution time-of-flight mass spectrometry (HR-TOF/MS) with colorized fuzzy difference (CFD) method was used to investigate the effect of sulfur-fumigation on the volatile components from Radix Angelicae Sinensis. Twenty-five compounds that were found in sun-dried samples disappeared in sulfur-fumigated samples. Seventeen volatile components including two sulfur-containing compounds were newly generated for the first time in volatile oils of sulfur-fumigated Radix Angelicae Sinensis. The strategy can be successfully applied to rapidly and holistically discriminate sun-dried and sulfur-fumigated Radix Angelicae Sinensis. GCxGC-HR-TOF/MS based CFD is a powerful and feasible approach for the global quality evaluation of Radix Angelicae Sinensis as well as other herbal medicines.

Processing impact on volatile compounds profile in higholeic and normal peanut oil

With the improvement of living quality, high-oleic peanuts have drawn people’s attention. Increasing oleic acid content of peanut oil should be desired for improving shelf life and potential health benefits. The flavor is among the most important quality attributes for commercial acceptance of peanuts products. The volatile components of high-oleic pea-nuts oil and normal-oleic lines were compared in this research. First, volatile components of peanut oils were analyzed and identified by solid-phase microextraction/gas chroma- tography/mass spectrometry （SPME/GC/MS）. Then principal components analysis （PCA） was used to identify principal volatile components in peanut oils of different cultivars fo卜 lowing three different processing methods, including roasting, boiling and roasting, and roasting by microwave-assisted. The results showed that there were obvious differences of the volatile components between high-oleic and normal peanut oils. Among different pro-cessing method of peanuts, there was no clear separation on volatile components observed between roasting and boiling and roasting by microwave-assisted. Moreover, the same genotype had the similar flavor characteristic. Different processing methods had no signifi-cant effect on volatile components in peanut oils.

Application of a Quartz Crystal Microbalance (QCM) System Coated with Chromatographic Adsorbents for the Detection of Olive Oil Volatile Compounds

A sensor based on the technique of a piezoelectric quartz crystal microbalance (QCM) is analyzed for the detection of six organic volatile compounds with high olive oil sensory significance, such as hexanal, acetic acid, Z-3-hexenyl acetate, undecane, 1-octen-3-ol and 2-butanone. Four sample concentrations have been exposed to each QCM sensor constructed. The detection system is based on the sample adsorption on the forty sensing films coated at the surfaces of forty AT-cut gold-coated quartz crystals. Each sensing film has been prepared with different solution concentrations of ten materials, usually used as chromatographic sta-tionary phases. Sensing film coating process shows excellent repeatability, with coefficient values less than 0.50%. The frequency shifts of the piezoelectric crystals due to the adsorption of the volatile compounds have been measured as sensor responses, using a static measurement system. The results show that only five QCM sensors, with high sensitivity values, are enough to the detection of the volatile compounds studied. Therefore, the developed detection system presented herein provides a rapid identification of organic volatile compounds with elevated olive oil sensory connotation and it could be a substitute technique to the analytical methods normally used for the analysis of the olive oil flavor.

Volatile Organic Compounds in Crude Coconut and Petroleum Oils in Nigeria

Analysis of Volatile Organic Compounds (VOCs) in crude coconut and petroleum oils from Nigeria is reported. Using head-space gas chromatography with a flame ionization detector and mass spectrometer, 8 VOCs were found in crude coconut oil and 29 VOCs were identified in crude petroleum oil. Crude coconut oil contained two aromatic, two nitrogenated, and four oxygenated compounds. Alkane, alkene, alkyne, halogenated, and sulfur compounds were absent in crude coconut oil but not in crude petroleum oil. The same observation held true for naphthalene. Conversely, benzofuran was absent in crude petroleum oil but was present in crude coconut oil at a concentration of 1.38 part-per-billion (ppb). The most concentrated VOC in crude coconut oil was dodecanoic acid at 9.98 ppb and that of crude petroleum oil was toluene at 12.61 ppb. Total VOC concentrations in crude coconut and petroleum oils are 20.49 and 87.46 ppb, respectively. These results are helpful in characterizing the chemical signature of Nigerian crude coconut oil for potential forensics use or in biofuel research.

Assessment of Uinta Basin Oil and Natural Gas Well Pad Pneumatic Controller Emissions

In the fall of 2016, a field study was conducted in the Uinta Basin Utah to improve information on oil and natural gas well pad pneumatic controllers (PCs) and emission measurement methods. A total of 80 PC systems at five oil sites (supporting six wells) and three gas sites (supporting 12 wells) were surveyed, and emissions data were produced using a combination of measurements and engineering emission estimates. Ninety-six percent of the PCs surveyed were low actuation frequency intermittent vent type. The overall whole gas emission rate for the study was estimated at 0.36 scf/h with the majority of emissions occurring from three continuous vent PCs (1.1 scf/h average) and eleven (14%) malfunctioning intermittent vent PC systems (1.6 scf/h average). Oil sites employed, on average 10.3 PC systems per well compared to 1.5 for gas sites. Oil and gas sites had group average PC emission rates of 0.28 scf/h and 0.67 scf/h, respectively. This difference was due in part to differing site selection procedures used for oil and gas sites. The PC system types encountered, the engineering emissions estimate approach, and comparisons to measurements are described. Survey methods included identification of malfunctioning PC systems and emission measurements with augmented high volume sampling and installed mass flow meters, each providing a somewhat different representation of emissions that are elucidated through example cases.

Composition and origin of molecular compounds in the condensate oils of the Dabei gas field, Tarim Basin, NW China

The Dabei gas field in the Kuqa Depression of the Tarim Basin is the most complex and deep continental condensate gas field in China. Comprehensive two-dimensional gas chromatography?time of flight mass spectrometer (GC×GC-TOFMS) analysis was conducted on five condensate oil samples from this field. The results show that the samples have n-alkane series in complete preservation and rich adamantanes. According to the methyladamantane index, the condensate oil is the product of the source rock with vitrinite reflectance (Ro) of 1.3%–1.6%. According to the gas maturity calculated through carbon isotope and vitrinite reflectance, the natural gas is corresponding to Ro of 1.3%–1.7%, reflecting that the natural gas and condensate oil are basically formed during the same period at the high maturity stage of source rock. The Dabei gas field has favorable geological conditions for hydrocarbon accumulation: thick salt rock in the Paleogene acts as a regional high-quality caprock directly overlying the high-quality sandstone reservoir of the Cretaceous, the coal source rocks have high hydrocarbon generation intensity and provide continuous oil and gas, and the subsalt thrust structures develop in rows with rich faults, providing migration pathways for oil and gas migration. These factors together controlled the formation of the Dabei gas field.

Erratum to “Assessment of Uinta Basin Oil and Natural Gas Well Pad Pneumatic Controller Emissions” [Journal of Environmental Protection, 2017, 8, 394-415]

In the fall of 2016, a field study was conducted in the Uinta Basin Utah to improve information on oil and natural gas well pad pneumatic controllers (PCs) and emission measurement methods. A total of 80 PC systems at five oil sites (supporting six wells) and three gas sites (supporting 12 wells) were surveyed, and emissions data were produced using a combination of measurements and engineering emission estimates. Ninety-six percent of the PCs surveyed were low actuation frequency intermittent vent type. The overall whole gas emission rate for the study was estimated at 0.36 scf/h with the majority of emissions occurring from three continuous vent PCs (1.1 scf/h average) and eleven (14%) malfunctioning intermittent vent PC systems (1.6 scf/h average). Oil sites employed, on average 10.3 PC systems per well compared to 1.5 for gas sites. Oil and gas sites had group average PC emission rates of 0.28 scf/h and 0.67 scf/h, respectively. This difference was due in part to differing site selection procedures used for oil and gas sites. The PC system types encountered, the engineering emissions estimate approach, and comparisons to measurements are described. Survey methods included identification of malfunctioning PC systems and emission measurements with augmented high volume sampling and installed mass flow meters, each providing a somewhat different representation of emissions that are elucidated through example cases.

Study on the Chromatographic Fingerprint of Volatile Constituents from Acacia Honey

[Objective] The experiment aimed to study chromatographic fingerprint in volatile components of acacia honey and provide scientific evaluation and effective control on quality of acacia honey.[Method] Using solid-phase microextraction method to separate and detect volatile components and construct chromatographic fingerprint.[Result] The honey was preheated for 15 min in water bath at 40 ℃ and solid-phase microextraction 85 μmPA was used to extract in overhead air about 30 min,then put it into the injector and desorpted 3 min,which is in 230 ℃.The Supelco WaxTM10 30 m×0.25 mm×0.25 μm column and gradient heating program was the best method to separate volatile components from honey.83 fingerprint peaks were constructed,among which 17 common fingerprint peaks were comprised of chromatographic fingerprint of volatile components of acacia honey.[Conclusion] The chromatographic fingerprint could provide reference for quality control of acacia honey.