QSRR Study of GC Retention Indices of Volatile Compounds Emitted from Mosla chinensis Maxim by Multiple Linear Regression

The volatile compounds emitted from Mosla chinensis Maxim were analyzed by headspace solid‐phase microextraction (HS‐SPME) and headspace liquid‐phase microextraction (HS‐LPME) combined with gas chromatography‐mass spectrometry (GC‐MS). The main volatiles from Mosla chinensis Maxim were studied in this paper. It can be seen that 61 compounds were separated and identified. Forty‐nine volatile compounds were identified by SPME method, mainly including myrcene, α‐terpinene, p‐cymene, (E)‐ocimene, thymol, thymol acetate and (E)‐β‐farnesene. Forty‐five major volatile compounds were identified by LPME method, including α‐thujene, α‐pinene, camphene, butanoic acid, 2‐methylpropyl ester, myrcene, butanoic acid, butyl ester, α‐terpinene, p‐cymene, (E)‐ocimene, butane, 1,1‐dibutoxy‐, thymol, thymol acetate and (E)‐β‐farnesene. After analyzing the volatile compounds, multiple linear regression (MLR) method was used for building the regression model. Then the quantitative structure‐retention relationship (QSRR) model was validated by predictive‐ability test. The prediction results were in good agreement with the experimental values. The results demonstrated that headspace SPME‐GC‐MS and LPME‐GC‐MS are the simple, rapid and easy sample enrichment technique suitable for analysis of volatile compounds. This investigation provided an effective method for predicting the retention indices of new compounds even in the absence of the standard candidates.     

Speciation of inorganic and tetramethyltin by headspace solid‐phase microextraction and gas chromatography–mass spectrometry

A headspace solid‐phase microextraction (HS‐SPME) method coupled to GC‐MS was developed in order to determine trace levels of tetramethyltin (TeMT) and inorganic tin (iSn) after ethylation to tetraethyltin (TeET) in various matrices. The derivatization of iSn and the extraction of both TeMT and iSn as TeET were performed in one step. Sodium tetraethylborate (NaBEt₄) was used as derivatization agent and the volatile derivatives were absorbed on a PDMS‐coated fused silica fiber. The conditions for the HS‐SPME procedure were optimized in order to gain in repeatability and sensitivity. Several critical parameters of GC‐MS were also studied. The detection of TeMT and iSn as TeET peaks was performed by the SIM mode. The precision of the proposed method is satisfactory providing RSD values below 10% for both tin species and good linearity up to 10 μg/L. The developed method was successfully applied to the determination of tin species in several samples like canned fish, fish tissues, aquatic plants, canned mineral water and sea water. The proposed HS‐SPME‐GC‐MS method was proved suitable to monitor the concentration levels of toxic tin compounds in environmental and biological samples.     

Optimization of a novel headspace–solid‐phase microextraction–gas chromatographic method by means of a Doehlert uniform shell design for the analysis of trace level ethylene oxide residuals in sterilized medical devices

Medical devices sterilized by ethylene oxide (EtO) retain trace quantities of EtO residuals, which may irritate patients' tissue. Reliably quantifying trace level EtO residuals in small medical devices requires an extremely sensitive analytical method. In this research, a Doehlert uniform shell design was utilized in obtaining a response surface to optimize a novel headspace–solid‐phase microextraction–gas chromatographic (HS‐SPME‐GC) method developed for analyzing trace levels of EtO residuals in sterilized medical devices, by evaluating sterilized, polymer‐coated, drug‐eluting cardiovascular stents. The effects of four independent experimental variables (HS‐SPME desorption time, extraction temperature, GC inlet temperature and extraction time) on GC peak area response of EtO were investigated simultaneously and the most influential experimental variables determined were extraction temperature and GC inlet temperature, with the fitted model showing no evidence of lack‐of‐fit. The optimized HS‐SPME‐GC method demonstrated overall good linearity/linear range, accuracy, repeatability, reproducibility, absolute recovery and high sensitivity. This novel method was successfully applied to analysis of trace levels of EtO residuals in sterilized/aerated cardiovascular stents of various lengths and internal diameter, where, upon heating, trace EtO residuals fully volatilized into HS for extraction, thereby nullifying matrix effects. As an alternative, this novel HS‐SPME‐GC method can offer higher sensitivity compared with conventional headspace analyzer‐based sampling. Copyright © 2009 John Wiley & Sons, Ltd.     

Use of two different coating temperatures for a cold fiber headspace solid‐phase microextraction system to determine the volatile profile of Brazilian medicinal herbs

In this study, the experimental extraction conditions on applying headspace solid‐phase microextraction and cold fiber headspace solid‐phase microextraction (CF‐HS‐SPME) procedures to samples of six medicinal herbs commonly found in southern Brazil were optimized. The optimized conditions for headspace solid‐phase microextraction were found to be an extraction temperature of 60°C and extraction time of 40 min. For CF‐HS‐SPME, the corresponding values were 60°C and 15 min. In the case of the coating temperature for the CF‐HS‐SPME system, two approaches were investigated: (i) Temperature of 5°C applied during the whole extraction procedure; and (ii) the use of two fiber temperatures in the same extraction procedure with the aim of extracting the volatile and semivolatile compounds, the ideal condition being 60°C for the first 7.5 min and 5°C for the final 7.5 min. The three extraction procedures were compared. The CF‐HS‐SPME procedure had good performance only for the more volatile compounds whereas the strategy using two coating temperatures in the same procedure showed good performance for all compounds studied. It was also possible to determine the profile for the volatile fraction of each herb studied applying this technique followed by GC‐MS.     

Analysis of volatile oil composition of Citrus aurantium L. by microwave‐assisted extraction coupled to headspace solid‐phase microextraction with nanoporous based fibers

Nanoporous silica was prepared and functionalized with amino propyl‐triethoxysilane to be used as a highly porous fiber‐coating material for solid‐phase microextraction (SPME). The prepared nanomaterials were immobilized onto a stainless steel wire for fabrication of the SPME fiber. The proposed fiber was evaluated for the extraction of volatile component of Citrus aurantium L. leaves. A homemade microwave‐assisted extraction followed by headspace (HS) solid‐phase apparatus was used for the extraction of volatile components. For optimization of factors affecting the extraction efficiency of the volatile compounds, a simplex optimization method was used. The repeatability for one fiber (n = 4), expressed as RSD, was between 3.1 and 8.6% and the reproducibility for five prepared fibers was between 10.1 and 14.9% for the test compounds. Using microwave‐assisted distillation HS‐SPME followed by GC‐MS, 53 compounds were separated and identified in C. aurantium L., which mainly included limonene (62.0%), linalool (7.47%), trans‐β‐Ocimene (3.47%), and caryophyllene (2.05%). In comparison to a hydrodistillation method, the proposed technique could equally monitor almost all the components of the sample, in an easier way, which was rapid and required a much lower amount of sample.     

Effect of sample matrix on sensitivity of mercury and methylmercury quantitation in human urine,saliva, and serum using GC‐MS

A rapid and sensitive method has been developed for the simultaneous determination of monomethylmercury (MMHg) and inorganic mercury (iHg) in human body fluids. The procedure is based on in situ derivatization of MMHg and iHg with sodium tetraethylborate (NaBEt₄) directly in aqueous solutions followed by headspace solid phase microextraction (HS‐SPME). The extracted species from spiked human urine, saliva, and serum are separated by capillary gas chromatography and detected by quadrupole MS (GC‐MS). The optimization of the HS‐SPME conditions like temperature, sample volume, extraction duration, and amount of alkylation agent, was performed in urinary solutions and aqueous solutions similarly buffered. The gas chromatographic conditions like injection temperature, helium flow rate, temperature program, and pressure conditions were also optimized. The recovery was ranged between 85 and 96% for MMHg and 88 and 98% for iHg. The LODs achieved were 10 and 15 ng/L for iHg and MMHg in urine, respectively, 54 and 60 ng/L for iHg and MMHg in saliva, respectively, and 61 and 81 ng/L for iHg and MMHg in serum, respectively. The RSD was ranged between 6.2 and 9.2% for MMHg and 5.0 and 8.2% for iHg.     

Classification of bacteria by simultaneous methylation–solid phase microextraction and gas chromatography/mass spectrometry analysis of fatty acid methyl esters

Direct methylation and solid-phase microextraction (SPME) were used as a sample preparation technique for classification of bacteria based on fatty acid methyl ester (FAME) profiles. Methanolic tetramethylammonium hydroxide was applied as a dual-function reagent to saponify and derivatize whole-cell bacterial fatty acids into FAMEs in one step, and SPME was used to extract the bacterial FAMEs from the headspace. Compared with traditional alkaline saponification and sample preparation using liquid–liquid extraction, the method presented in this work avoids using comparatively large amounts of inorganic and organic solvents and greatly decreases the sample preparation time as well. Characteristic gas chromatography/mass spectrometry (GC/MS) of FAME profiles was achieved for six bacterial species. The difference between Gram-positive and Gram-negative bacteria was clearly visualized with the application of principal component analysis of the GC/MS data of bacterial FAMEs. A cross-validation study using ten bootstrap Latin partitions and the fuzzy rule building expert system demonstrated 87 ± 3% correct classification efficiency.      

Discrimination between 2AP producing and non‐producing rice rhizobacterial isolates using volatile profiling: a chemometric approach

2‐Acetyl‐1‐pyrroline (2AP) is known as a principal basmati aroma compound. The present study aims at discriminating rhizobacteria isolated from soils cultivated with basmati and non‐basmati rice for long duration. Volatile profiling was used as marker to discriminate the rhizobacterial isolates. Quantification of 2AP and other volatile compounds (VCs) produced by rhizobacteria was undertaken using HS‐SPME coupled with GC‐MS. Chemometrics tools such as hierarchical cluster analysis (HCA), principle component analysis (PCA) and multi dimensional scaling (MDS) were applied for volatile profiling of different isolates. Results showed significant discrimination of all 2AP producing (AP‐P) and non‐producing rhizobacterial isolates (AP‐NP) on the basis of their VC profile. This was validated by bacterial identification data as well. The frequency distribution for 2AP levels indicates that basmati isolates had higher frequency for 2AP production as compared to non‐basmati control. AP‐P and AP‐NP isolates have different VC profiling pattern irrespective of their origin. These isolates were found belonging to different groups when identified using 16S rDNA sequencing data. Chemometric analysis (PCA, HCA and MDS) helped to identify volatiles, which could be used as biomarker in discriminating the AP‐P and AP‐NP isolates. VC pattern of rhizobacteria could be used as volatile markers to distinguish between AP‐P and AP‐NP rhizobacterial isolates. Copyright © 2015 John Wiley & Sons, Ltd.     

Characterization of volatile substances in apples from Rosaceae family by headspace solid‐phase microextraction followed by GC‐qMS

The volatile composition of different apple varieties of Malus domestica Borkh. species from different geographic regions at Madeira Islands, namely Ponta do Pargo (PP), Porto Santo (PS), and Santo da Serra (SS) was established by headspace solid‐phase microextraction (HS‐SPME) procedure followed by GC‐MS (GC‐qMS) analysis. Significant parameters affecting sorption process such as fiber coating, extraction temperature, extraction time, sample amount, dilution factor, ionic strength, and desorption time, were optimized and discussed. The SPME fiber coated with 50/30 μm divinylbenzene/carboxen/PDMS (DVB/CAR/PDMS) afforded highest extraction efficiency of volatile compounds, providing the best sensitivity for the target volatiles, particularly when the samples were extracted at 50°C for 30 min with constant magnetic stirring. A qualitative and semi‐quantitative analysis between the investigated apple species has been established. It was possible to identify about 100 of volatile compounds among pulp (46, 45, and 39), peel (64, 60, and 64), and entire fruit (65, 43, and 50) in PP, PS, and SS apples, respectively. Ethyl esters, terpenes, and higher alcohols were found to be the most representative volatiles. α‐Farnesene, hexan‐1‐ol and hexyl 2‐methylbutyrate were the compounds found in the volatile profile of studied apples with the largest GC area, representing, on average, 24.71, 14.06, and 10.80% of the total volatile fraction from PP, PS, and SS apples. In PP entire apple, the most abundant compounds identified were α‐farnesene (30.49%), the unknown compound m/z (69, 101, 157) (21.82%) and hexyl acetate (6.57%). Regarding PS entire apple the major compounds were α‐farnesene (16.87%), estragole (15.43%), hexan‐1‐ol (10.94), and E‐2‐hexenal (10.67). α‐Farnesene (30.3%), hexan‐1‐ol (18.90%), 2‐methylbutanoic acid (4.7%), and pentan‐1‐ol (4.6%) were also found as SS entire apple volatiles present in a higher relative content. Principal component analysis (PCA) of the results clustered the apples into three groups according to geographic origin. Linear discriminant analysis (LDA) was performed in order to detect the volatile compounds able to differentiate the three kinds of apples investigated. The most important contributions to the differentiation of the PP, PS, and SS apples were ethyl hexanoate, hexyl 2‐methylbutyrate, E,E‐2,4‐heptadienal, p‐ethyl styrene, and E‐2‐hexenal.     

Comparative analysis of volatile constituents between recipe jingfangsan and its single herbs by GC‐MS combined with alternative moving window factor analysis method

Comparative analysis of volatile constituents between recipe jingfangsan and its single herbs was performed by GC‐MS combined with alternative moving window factor analysis (AMWFA), a new chemometric resolution method. Identification of the compounds was also assisted by comparison of temperature‐programmed retention indices (PTRIs) on the OV‐1 column with authentic samples. In total, 36, 29, and 42 volatile components in essential oil of Herba schizonepetae (HS), Radix saposhnikoviae (RS), and the recipe were respectively determined qualitatively and quantitatively, accounting for 81.80, 82.62 and 85.98% total contents of volatile oil of HS, RS, and the recipe respectively. Analysis by the method of AMWFA indicates that there are 22 common volatile constituents between the recipe and single herbal medicine HS, and 14 common volatile constituents between the recipe and single herb medicine RS. The experimental results also show that the volatile components of the recipe in number are almost addition of that of two single herbal medicines HS and RS, and are mainly from the single herbal medicine HS.     

碳纳米管顶空固相微萃取测定水中的多溴联苯醚

建立了顶空固相微萃取联结气相色谱-电子捕获检测器（HS-SPME-GC-ECD）测定水中多溴联苯醚的方法。制作了多壁碳纳米管涂层固相微萃取探头。优化了萃取时间,萃取温度,搅拌速度,顶空体积,溶液的pH,离子强度及有机溶剂等影响萃取效率的各种因素。比较了室温和100 ℃顶空萃取和直接萃取的效率。结果表明,室温下直接萃取比顶空萃取的效率高2-4倍,而在100 ℃时顶空萃取比直接萃取的效率高1-8倍。除BDE-154外,无论直接萃取还是顶空萃取,100 ℃时的萃取效率均高于室温。方法的线性范围50-1600 ng/L,相关系数为0.995-0.998,5种多溴联苯醚的最低检出限（S/N=3）为1.14-16.25 ng/L,相对标准偏差（RSD%,n=5）小于10%。本方法用于真实水样的测定,回收率为74.2%-98.7%。     

Solid-phase microextraction method for carbon isotopic analysis of volatile carboxylic acids in human plasma by gas chromatography/combustion/isotope ratio mass spectrometry

A new analytical method is described for the determination of the physiological concentration and low-level enrichment of (13)C-short-chain volatile organic acids (SCVAs) (e.g. (13)C-acetate and (13)C-butyrate) in human plasma. This two-step method involves solid-phase microextraction (SPME) coupled to gas chromatography/combustion/isotope ratio mass spectrometry (GC/C/IRMS) without any organic solvents or derivatizing agents. Two SCVA extraction methods were compared using a carboxen/polydimethylsiloxane fiber: headspace sampling (HS) and liquid sampling (LS) SPME. The influences of extraction temperature and time were tested to optimize the adsorption of SCVAs onto the fiber. The comparison of the peak area responses of the acids in the two adsorption methods showed better sensitivity in the human physiological concentration range in the LS mode than in the HS mode.The accuracy of isotopic enrichment measurement was determined using plasma spiked with (13)C-acetate and (13)C-butyrate solution from 0 to 1 mol percent excess (MPE). The linearity and repeatability (RSD < 5%) were measured in LS mode. Plasma SCVA concentrations were also determined relative to 3-methylvalerate (internal standard). Linearity and repeatability were observed from 0 to 400 microM for acetate, from 0 to 20 microM for propionate, and from 0 to 10 microM for butyrate. This method was also used to determine plasma acetate production obtained from lactulose (an undigestible disaccharide) fermentation in one healthy volunteer over 3 h. The acetate concentration increased twofold, 2 h after oral lactulose intake. These results are in agreement with the data obtained by GC/MS in healthy volunteers and obese adults following a lactulose intake by using higher amounts of labelled tracers.SPME coupled with GC/C/IRMS can be used to analyze (13)C-SCVAs at low enrichment (<0.5 MPE) within the physiological concentration measured in human plasma.     

Optimization of headspace sampling using solid‐phase microextraction for chloroanisoles in cork stoppers and gas chromatography–ion‐trap tandem mass spectrometric analysis

In a study aiming to characterize cork off‐flavour for quality control purposes, chloroanisoles were extracted and identified from cork stoppers by means of solid‐phase microextraction (SPME)–gas chromatography–ion‐trap mass spectrometry (GC–ITMS). An experimental design procedure was used to investigate the effects of some experimental parameters on the SPME of 2,4‐dichloroanisole, 2,6‐dichloroanisole, and 2,4,6‐trichloroanisole from cork stoppers by using a Carboxen‐PDMS 75 μm fibre. Variables such as extraction temperature, extraction time, and percentage of ethanol added to the matrix were optimized to improve extraction efficiency of chloroanisoles onto SPME fibre. Instrumental analysis was performed by GC–ITMS in the MS/MS mode. Preliminary analyses on standard solutions allowed selection of the appropriate ionization mode (i. e. electron impact or chemical ionization), providing for each analyte the highest instrumental response. In order to find polynomial functions describing the relationships between variables and responses, the analytical responses, i.e. the chromatographic peak areas, were processed by using the backward multiple regression analysis. For all the analytes the operating conditions providing the highest extraction yield inside the experimental domain considered were found.     

Application of solid-phase microextraction and gas chromatography-mass spectrometry for the determination of chlorophenols in leather

This paper proposes a new analytical procedure based on the headspace solid‐phase microextraction (HS‐SPME) technique and gas chromatography‐selected ion monitoring‐mass spectrometry (GC‐SIM‐MS) for the determination of 16 phenols extracted from leather samples. The optimized conditions for the HS‐SPME were obtained through two experimental designs – a two‐level fractional factorial design followed by a central composite design – using the commercial SPME fiber polyacrylate 85 μm (PA). The best extraction conditions were as follows: 200 μL of derivatizing agent (acetic anhydride), 20 mL of saturated aqueous NaCl solution and extraction time and temperature of 50 min and 75°C, respectively. All optimized conditions were obtained with fixed leather sample mass (250 mg), vial volume (40 mL) and phosphate buffer pH (12) and concentration (50 mmol/L). Detection limits ranging from 0.03 to 0.20 ng/g, and relative standard deviation (RSD) lower than 10.23% (n=6) for a concentration of 800 ng/g (chlorophenols) and 1325 ng/g (2‐phenylphenol) in the splitless mode were obtained. The recovery was studied at three concentration levels by adding different amounts of phenols to the leather sample and excellent recoveries ranging from 90.0 to 107.2% were obtained. The validated method was shown to be suitable for the quantification of phenols in leather samples, as it is simple, relatively fast and sensitive.     

Analytical bias among different gas chromatographic approaches using standard BTX gases and exhaust samples

In this study, the analytical compatibility of the gas chromatographic (GC) approach was evaluated through a cross‐calibration exercise. To this end, three aromatic volatile organic compounds (VOCs: benzene, toluene, and p‐xylene (BTX)) were simultaneously analyzed with four individual instrumental setups (type I = GC with MS plus solid phase microextraction (SPME) method, II = GC with flame ionization detection (FID) plus SPME, III = fast GC‐FID plus SPME, and IV = GC‐FID plus air server/thermal desorption (AS/TD) method). A comparison of basic quality assurance (QA) data revealed considerable differences in DL values among the methods with moderate variabilities in the intercompound sensitivity. In light of the differences in detection properties, the analytical bias involved for each methodological approach was assessed by the relative relationship between analytes and basic operating conditions. The results suggest that the analysis of environmental samples at ultra‐low concentration levels (at or below ppb level) can be subject to diverse sources of bias. Although detection properties of target compounds seem to be affected by the combined effects of various factors, changes in the sample concentration levels were seen to be the most consistent under the experimental setups analyzed in this study.     

Metabolite analysis in Curcuma domestica using various GC‐MS and LC‐MS separation and detection techniques

The metabolic profile of polar (methanol) and non‐polar (hexane) extracts of Curcuma domestica, a widely used medicinal plant, was established using various different analytical techniques, including GC‐FID, GC‐MS, HR‐GC‐MS and analytical HPLC‐ESI‐MS/MS by means of LTQ‐Orbitrap technology. The major non‐volatile curcuminoids curcumin, demethoxycurcumin and bisdemethoxycurcumin were identified when their chromatographic and precursor ion masses were compared with those of authentic standard compounds. In this paper we describe for the first time a GC/MS‐based method for metabolic profiling of the hydrophilic extract. We also identified 61 polar metabolites as TMS derivatives. Copyright © 2009 John Wiley & Sons, Ltd.     

Application of gas-sensor array technology for detection and monitoring of growth of spoilage bacteria in milk: A model study

The aim of this study was to develop a novel, rapid system for detection and monitoring of growth of undesirable bacteria in food using gas-sensor array technology. Three spoilage bacteria isolated from a cheese-processing hall were identified as Serratia marcescens, Serratia proteamacufans and Pseudomonas putida. The growth of these bacteria in milk was investigated using a commercial solid state based gas-sensor array system. On the basis of the temporal sensor readings of the pure cultures, bacterial growth could be monitored and the individual strains identified and followed throughout the complete growth cycle in both single and mixed culture. The gas-sensor signals could be used as early indicators of the onset of bacterial growth. Start detection of volatile bacterial metabolites coincided with the start of the exponential growth phase taking place around 7 h after inoculation and corresponding to bacterial numbers of 10⁴ (cfu/ml). The results were confirmed by comparing the gas profiles with the cell counts and by headspace gas chromatography mass spectrometry (GC/MS) of volatile microbial metabolites. High correlation (r > 0.90, p < 0.001) was found between the gas-sensor readings and major secondary volatile metabolites. Using the sensor readings, cell numbers of single strain cultures could be predicted with an error of less than 5%. The results show that it is possible to monitor growth of individual strains of spoilage bacteria in a mixed culture in milk on the basis of the type and amount of volatile compounds which they produce, using a gas-sensor array system. The system thus affords possibilities for further development for quick, more accurate and full scale determinations of shelf life, the design of spoilage indicators, rapid identification of undesired microorganisms and rapid measurements of spoilage.     

Time‐of‐flight secondary ion mass spectrometry and gas chromatography–mass spectrometry studies of alkanethiol self‐assembled monolayers on nanoporous gold surfaces

The dimerization of alkanethiol mixtures (hexanethiol, octanethiol, and dodecanethiol) to form self‐assembled monolayers (SAMs) from headspace on nanoporous gold surfaces was studied for the first time using gas chromatography (GC/MS) and time‐of‐flight secondary ion mass spectrometry (TOF‐SIMS). The nanoporous gold surfaces were obtained by an acidic etching of a 585‐gold alloy. Field emission scanning electron microscopy (FE‐SEM) was utilized to study the change of the surface geometry and porosity of the gold surfaces before and after etching. Alkanethiols were deposited from the vapor phase above the thiol solutions (headspace) on nanoporous gold plates and nanoporous gold solid‐phase vmicroextraction (SPME) fibers. The nanoporous gold substrates were analyzed by TOF‐SIMS and GC/MS, respectively. The TOF‐SIMS spectra exhibited various gold–sulfur ion clusters and specific peaks related to the adsorption of thiols such as deprotonated monomers, thiolate–Au, dimers (e.g., dialkyl sulfides–Au and dialkyl disulfides–Au). The GC/MS analysis of headspace extractions of alkanethiol mixtures by nanoporous gold SPME fibers showed a high extraction efficiency of alkanethiol, dialkyl sulfide, and dialkyl disulfide when compared with the commercial SPME fibers (DVB‐CAR‐PDMS and CAR‐PDMS). Different GC/MS optimization factors were studied including the extraction time and desorption temperature.     

Comparative Analysis of the Volatile Components in the Fresh Roots and Rhizomes of Curcuma wenyujin by Static Headspace Gas Chromatography Mass Spectrometry

Static headspace GC-MS method coupled with H/D exchange was firstly developed to determine and identifythe volatile components in the fresh root and rhizome of Curcuma wenyujin.The TIC chromatograms of 3 batchesof fresh roots harvested at different time showed significant difference in the volatile components:the constitutionwas the same but the content of them was different.More than 60 volatile components in fresh roots(Root of C.wenyujin)and rhizomes(Rhizome of C.wenyujin)of C.wenyujin were detected,of which 51 and 48 volatile com-ponents were identified respectively.The fresh roots and rhizomes of C.wenyujin were found to have the similarvolatile components.The contents of these components were calibrated by the response of β-elemene.In addition,the principal active component,β-elemene,was further confirmed and relatively quantified by its standard.γ-terpinene showed obvious allylic hydrogen/deuterium exchange using deuterium oxide which gave a new methodto identify some compounds containing allylic hydrogen.At the same time,the active hydrogen compounds werealso further confirmed.The results show that HS-GC-MS method is a fast,simple and efficient way for the analysisof volatile components from medical plants.