Determination of 8 Diuretics and Probenecid in Human Urine by Gas Chromatography-Mass Spectrometry: Confirmation Procedure

A fast and sensitive method for determination of 8 diuretics (acetazolamide, bendroflumethiazide, bumetanide, chlorthalidone, furosemide, hydrochlorothiazide, metolazone, triamterene) and masking agent (probenecid) in human urine using gas-chromatography with mass spectrometric detection is described. The extraction of the substances as function of the nature of organic solvent, mixing time and pH of aqueous phase was studied. The tandem mass spectrometry was used to increase selectivity of diuretics determination due to elimination of background interferences. Fragmentation reactions were studied for each compound and their collision energies were optimized to obtain the best selectivity. The results of method’s validation demonstrate its suitability in routine analysis for confirmation purposes.

Occurrence of <i>N</i>-Acyl Homoserine Lactones in Extracts of Bacterial Strain of <i>Pseudomonas aeruginosa</i>and in Sputum Sample Evaluated by Gas Chromatography–Mass Spectrometry

This study presents a fast, accurate and sensitive technique using gas chromatography-mass spectrometry (GC-MS) for the identification and quantification of N-acyl homoserine lactones (AHLs) in the extracts of bacterial strain of Pseudomonas aeruginosa and sputum sample of a cystic fibrosis patient. This method involves direct separation and determination of AHLs by using GC-MS as simultaneous separation and characterization of AHLs were possible without any prior derivatiza-tion. Electron ionization resulted in a common fragmentation pattern with the most common fragment ion at m/z 143 and other minor peaks at 73, 57 and 43. The limit of detection for N-butanoyl, N-hexanoyl, N-octanoyl, N-decanoyl, N-dodecanoyl and N-tetradecanoyl homoserine lactones was 2.14, 3.59, 2.71, 2.10, 2.45 and 2.34 μg/L, respectively. The presence of AHLs in the culture of P. aeruginosa strain and spu-tum of a cystic fibrosis patient was achieved in selected ion monitoring (SIM) mode by using the prominent fragment at m/z 143.

The Detection of THCA Using 2-Dimensional Gas Chromatography-Tandem Mass Spectrometry in Human Fingernail Clippings: Method Validation and Comparison with Head Hair

Marijuana use as well as abuse is a significant public health and public safety concern in the United States and using hair to identify marijuana users and abusers has been gaining acceptance in a number of venues including workplace, court ordered, and substance abuse treatment monitoring. After the presentation of a fully validated 2-dimensional gas chromatography-tandem mass spectrometry method for the detection of 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCA), the chief metabolite of the main psychoactive compound in marijuana, Δ9-tetrahydrocannabinol (THC), we evaluated the usefulness of fingernail clippings as an alternative specimen type to hair by the analysis of a set of 60 matched pairs of head hair and fingernail clippings. The limit of detection was 10 fg/mg, the limit of quantitation was 20 fg/mg, and the assay was linear from 20 fg/mg to 500 fg/mg. The intra- and inter-assay imprecision and bias studies at 4 different concentrations (50, 100, 500, and 1000 fg/mg) were acceptable where all % Target observations were within 16% of their expected concentrations and all %CV calculations were less than 13.5%. THCA was detectable in more fingernail specimens (53.3%) than hair specimens (46.7%) and the mean concentrations in nails were on average 4.9 times higher than in hair (1813 fg/mg and 364 fg/mg, respectively). The THCA concentrations in hair and nail were strongly associated (r = 0.974, P < 0.01, n = 60) and the association was significant. The study demonstrated that fingernail clippings are a suitable alternative specimen type to hair to monitor for marijuana use and abuse.

Pyrolysis-Gas Chromatography/Mass Spectrometry for Microstructure and Pyrolysis Pathway of Polyester-Polyether Multiblock Copolymer

The composition and sequence distribution of monomeric units in polyester polyether multiblock copolymer were studied by pyrolysis? gas chromatography (PGC) and pyrolysis gas chromatography/mass spectrometry (PGC/MS). PGC was applied to study the F t curve of the multiblock copolymer and PGC/MS was used to separate and identify the pyrolyzates. DTA experiment was used to study the decomposition temperature. The results show that the beginning point of elastomer’s decomposition was about 300?℃ and the decomposition temperature of most of the sample was 550?℃. Many pyrolyzates were produced because of the breaking of weak bonds in the sample. The possible microstructure was verified and the pyrolysis pathway of the copolymer was investigated.

Metabolomics of gastric cancer metastasis detected by gas chromatography and mass spectrometry

AIM:To elucidate the underlying mechanisms of metastasis and to identify the metabolomic markers of gastric cancer metastasis.METHODS:Gastric tumors from metastatic and nonmetastatic groups were used in this study.Metabolites and different metabolic patterns were analyzed by gas chromatography,mass spectrometry and principal components analysis (PCA),respectively.Differentiation performance was validated by the area under the curve (AUC) of receiver operating characteristic curves.RESULTS:Twenty-nine metabolites were differentially expressed in animal models of human gastric cancer.Of the 29 metabolites,20 were up-regulated and 9 were down-regulated in metastasis group compared to non-metastasis group.PCA models from the metabolite profiles could differentiate the metastatic from the nonmetastatic specimens with an AUC value of 1.0.These metabolites were mainly involved in several metabolic pathways,including glycolysis (lactic acid,alaline),serine metabolism (serine,phosphoserine),proline metabolism (proline),glutamic acid metabolism,tricarboxylic acid cycle (succinate,malic acid),nucleotide metabolism (pyrimidine),fatty acid metabolism (docosanoic acid,and octadecanoic acid),and methylation(glycine).The serine and proline metabolisms were highlighted during the progression of metastasis.CONCLUSION:Proline and serine metabolisms play an important role in metastasis.The metabolic profiling of tumor tissue can provide new biomarkers for the treatment of gastric cancer metastasis.

Gas chromatography/mass spectrometry based metabolomic study in a murine model of irritable bowel syndrome

AIM To study the role of microbial metabolites in the modulation of biochemical and physiological processes in irritable bowel syndrome(IBS).METHODS In the current study, using a metabolomic approach, we analyzed the key metabolites differentially excreted in the feces of control mice and mice with IBS, with or without Clostridium butyricum(C. butyricum) treatment. C57 BL/6 mice were divided into control, IBS, and IBS + C. butyricum groups. In the IBS and IBS + C. butyricum groups, the mice were subjected to water avoidance stress(WAS) for 1 h/d for ten days. Gas chromatography/mass spectrometry(GC-MS) together with multivariate analysis was employed to compare the fecal samples between groups. RESULTS WAS exposure established an appropriate model of IBS in mice, with symptoms of visceral hyperalgesia and diarrhea. The differences in the metabolite profiles between the control group and IBS group significantly changed with the progression of IBS(days 0, 5, 10, and 17). A total of 14 differentially excreted metabolites were identified between the control and IBS groups, and phenylethylamine was a major metabolite induced by stress. In addition, phenylalanine metabolism was found to be the most relevant metabolic pathway. Between the IBS group and IBS + C. butyricum group, 10 differentially excreted metabolites were identified. Among these, pantothenate and coenzyme A(Co A) biosynthesis metabolites, as well as steroid hormone biosynthesis metabolites were identified as significantly relevant metabolic pathways.CONCLUSION The metabolic profile of IBS mice is significantly altered compared to control mice. Supplementation with C. butyricum to IBS mice may provide a considerable benefit by modulating host metabolism.

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.

Analyzing crude oils from the Junggar Basin(NW China) using comprehensive two-dimensional gas chromatography coupled with time-of-flight mass spectrometry(GC×GC-TOFMS)

As a new technology of analyzing crude oils, comprehensive two-dimensional gas chromatography cou- pled with time-of-flight mass spectrometry （GCxGC- TOFMS） has received much research attention. Here we present a case study in the Junggar Basin of NW China. Results show that the hydrocarbons, including saturates and aromatics, were all well-separated without large co- elution, which cannot be realized by conventional one-dimensional GC-MS. The GC×GC technique is especially effective for analyzing aromatics and low-to-middle- molecular-weight hydrocarbons, such as diamondoids. The geochemical characteristics of crude oils in the study area were investigated through geochemical parameters extracted by GC×GC-TOFMS, improving upon the understanding obtained by GC-MS. Thus, the work here represents a new successful application of GC×GC- TOFMS, showing its broad usefulness in petroleum geochemistry.

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.

Structure Elucidation of a New Toxin from the Mushroom Cortinarius rubellus Using Gas Chromatography-Mass Spectrometry (GC-MS)

Cortinarius orellanus (Fries) and C. rubellus (Cooke),which were formerly also known as C. speciosissimus, are poisonous mushrooms containing the toxin orellanine and several degradation products of orellanine,includingorelline and orellinine. Mass intoxication by poisonous mushrooms was observed in Poland in 1952-1957 [1]. In 1957, the cause of these outbreaks was described by Grzymala as poisoning by a member of the Cortinarius family. The toxin orellanine was first isolated from C. orellanusby Grzymala in 1962;the chemical structure of orellanine was later determined to be 3,3',4,4'-tetrahydroxy-2,2'-bipyridine-N,N'-dioxide. Poisoning with C. orellanus and C. rubellus has a very specific character. The first symptoms of intoxication usually do not appear until 2-3 days after ingestion, but in some cases intoxication appears after three weeks. The target organ for the toxin is the kidney. Histologically, it is easy to record the specific damage. The presence of degradation products of orellanine in kidney can be confirmed chromatographically, suggesting that the cause of poisoning is orellanine. However, the presence of orellanine in the blood of intoxicated persons has not been directly detected. A specific model was developed by Brondz et al. for the detection of orellanine, orelline, and orellininein animal stomach fluids [2-4]. The hypothesis that the fungal toxin orellanine as a diglucoside can be transported from the digestive system by the blood to the kidney could not be supported. The toxin orellanine as a diglucoside is very unstable in an aqueous acidic environment.[i1]?However, in the present study, it was possible to record an additional substance in animal stomach fluids using GC-MSafter ingestion ofC. rubellus. This substance, which has been namedrubelline, is part of a toxic mixture inC. orellanusandC. rubellusand is closely related to orellanine. The structure of rubelline is more suitable than orellanine for absorptionfromthe digestive tract and for transport in the blood. The presented hypothesis is that rubellineis absorbed in the digestive tract and transportedin the blood to the kidney, where it is biotransformed to orellanine and accumulatedto toxic levels. The process of biotransformationis in itself also damaging for the kidney and liver.[i2]?GC-MS instrumentation enables the separation of substances in biological samples and in the extract fromC. rubellus. The GC-MS with SMB technique was used to record the mass ion and to record a detailed fragmentation picture.

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.

Coupling a Gas Chromatography Unit to an Inductively Coupled Plasma Mass Spectrometer

Although the eminent threat of a terrorist group detonating an improvised nuclear device (IND) in an urban environment is low, it is crucial that countries develop modern nuclear forensic capabilities to expedite response in a post-detonation scenario. In particular, new instruments need to be created to shorten dissolution time, expedite chemical separation, and improve forensic analysis of the nuclear melt glass that is created during the detonation of the device. To expedite this process, an instrument was designed to thermally couple a gas chromatograph (GC) to a time-of-flight inductively coupled plasma time-of-flight mass spectrometer (ICPTOFMS) In order to couple these two instruments, another instrument was designed to provide an isothermal atmosphere between the GC and TOFICPMS to expedite rapid gas separations processes. By using gas separations instead of the current wet chemistry processes, the required separation and analysis time of the melt glass significantly decreases. The new instrument would also provide a more detailed analysis of the elemental and isotopic composition of the melt glass. By completing these tasks simultaneously, this significantly decreases the required time to conduct these separations and improves the elemental and isotopic analysis.

Analysis of residual crosslinking agent content in UV cross-linked poly(ethylene oxide) hydrogels for dermatological application by gas chromatography

Acrylates have been widely used in the synthesis of pharmaceutical polymers. The quantitation of residual acrylate monomers is vital as they are strong irritants and allergens, but after polymerization, are relatively inert, causing no irritation and allergies. Poly(ethylene oxide)(PEO) hydrogels were prepared using pentaerythritol tetra-acrylate(PETRA) as UV crosslinking agent. A simple, accurate, and robust quantitation method was developed based on gas chromatographic techniques(GC), which is suitable for routine analysis of residual PETRA monomers in these hydrogels. Unreacted PETRA was initially identified using gas chromatography–mass spectrometry(GC–MS). The quantitation of analyte was performed and validated using gas chromatography equipped with a flame ionization detector(GC–FID). A linear relationship was obtained over the range of 0.0002%–0.0450%(m/m) with a correlation coefficient(r2)greater than 0.99. The recovery( 4 90%), intra-day precision(%RSD o 0.67), inter-day precision(%RSD o2.5%), and robustness(%RSD o1.62%) of the method were within the acceptable values. The limit of detection(LOD) and limit of quantitation(LOQ) were 0.0001%(m/m) and 0.0002%(m/m), respectively.This assay provides a simple and quick way of screening for residual acrylate monomer in hydrogels.

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.

Product Analysis of Supercritical Fischer-Tropsch Synthesis: Utilizing a Unique On-Line and Off-Line Gas Chromatographs Setup in a Bench-Scale Reactor Unit

The utilization of supercritical fluids (SCF) in the Fischer-Tropsch Synthesis (FTS) further complicates the hydrocarbon products identification and analysis process due to the dilution of hydrocarbon peaks by the predominant solvent peak. Therefore, in this project, a custom-made Gas Chromatography (GC) analysis system was designed and implemented to identify and quantify SCF-FTS products. The FTS products were identified using two different methods. The first was through retention time matching by injecting standard solutions, and the second was through the use of the GC/MS system. The quantification of CO and CH4 was achieved by using external standards, where the CO conversion was calculated by relating the peak area of CO to the peak area of an internal standard (argon) while the CH4 selectivity was calculated by relating the peak area of CH4 to that of CO. After setting and calibrating the GC system, two reaction conditions (gas phase: 240°C, 20 bar syngas with 2:1 H2:CO molar feed ratio and for the supercritical fluids FTS (SCF-FTS): 240°C, 65 bar with 20 bar syngas partial pressure and 2:1 H2:CO molar feed ratio) were used to compare the different FTS reaction media. The comparison between the gas phase FTS and the SCF-FTS showed the following: carbon monoxide conversion was improved by 14% in the SCF-FTS, while the hydrocarbon product profile SCF-FTS showed 78% reduction in light hydrocarbons (C1 - C4) products, 35% increase in middle distillates (C11 - C22) products compared to gas phase FTS. These improvements have resulted in higher chain growth probability for the SCF-FTS (α = 0.85) compared to the gas phase FTS (α = 0.76). These results are generally in agreement with previously reported enhancement in the SCF-FTS[1].

Sex Pheromone Components of the Female Black Cutworm Moth in China: Identification and Field Trials

The sex pheromone blend of a China strain of the black cutworm moth Agrotis ypsilon （Rottemberg） （Lepidoptera： Noctuidae） was investigated. Chemical analysis of pheromone gland extracts of 3-day-old females showed that individual isolated glands contained only very small amounts of pheromone. The high-resolution gas chromatography combined with mass spectrometry （GC-MS） analysis showed the presence of Cis-7-dodecenyl acetate （Z7-12：Ac, A）, Cis-9-tetradecenyl acetate （Z9-14：Ac, B）, Cis- 11-hexadecenyl acetate （Z 11 - 16 ：Ac, C）, Cis-8-dodecenyl acetate （Z8-12：Ac, E） and Cis-5-decenyl acetate （Z5-10：Ac, D） in biologically active pheromone gland extracts. An extract of one gland from a day 3 female gave the following values for the gland components： 0.245±0.098ng for Z7-12：Ac, 0.080±0.031ng for Z9-14：Ac, 0.089±0.033ng for Z11-16：Ac, 0.085±0.031ng for Z5-10：Ac, 0.105±0.065ng for Z8-12：Ac per female. The percentages of Z7-12：Ac, Z9-14：Ac, Z11-16：Ac, Z5-10：Ac and ZS-12：Ac in pheromone gland extracts from individual females were （meaniSE） 40.451±13.66, 13.176±5.279, 14.943±5.142, 14.392±6.10 and 17.225±9.792 respectively, and the percentages of Z7-12：Ac, Z9-14：Ac and Z11-16：Ac were 58.75±9.429, 18.91±7.539 and 22.34±7.209. Field trials indicated that each single component of sex pheromone was non-effective and captured no males. The lures baited with duality compound of AB （3 ： 1） had a certain attraction to males, the mean captured number was 2.6. The attraction ability of the lures baited with ternary compound of ABC （3 ： 1 ：1） to males added significantly, the mean captured number per trap was 7.40, which was 2.8 times of duality compound of AB （3 ： 1）. The contents of sex pheromone could obviously affect its capture ability to males, the mean captured number was the highest at the dosage of 200 μg.

Prediction of gastric cancer metastasis through urinary metabolomic investigation using GC/MS

AIM:To gain new insights into tumor metabolism and to identify possible biomarkers with potential diagnostic values to predict tumor metastasis.METHODS:Human gastric cancer SGC-7901 cells were implanted into 24 severe combined immune deficiency (SCID) mice,which were randomly divided into metastasis group (n=8),non-metastasis group (n=8),and normal group (n=8).Urinary metabolomic information was obtained by gas chromatography/mass spectrometry (GC/MS).RESULTS:There were significant metabolic differences among the three groups (t test,P < 0.05).Ten selected metabolites were different between normal and cancer groups (non-metastasis and metastasis groups),and seven metabolites were also different between non-metastasis and metastasis groups.Two diagnostic models for gastric cancer and metastasis were constructed respectively by the principal component analysis (PCA).These PCA models were confirmed by corresponding receiver operating characteristic analysis (area under the curve=1.00).CONCLUSION:The urinary metabolomic profile is different,and the selected metabolites might be instructive to clinical diagnosis or screening metastasis for gastric cancer.

Response to weaning and dietary L-glutamine supplementation:metabolomic analysis in piglets by gas chromatography/mass spectrometry

A novel metabolomic method based on gas chromatography/mass spectrometry （GC-MS） was applied to determine the metabolites in the serum of piglets in response to weaning and dietary L-glutamine （Gin） supplementation. Thirty-six 21-d-old piglets were randomly assigned into three groups. One group continued to suckle from the sows （suckling group）, whereas the other two groups were weaned and their diets were supplemented with 1% （w/w） Gin or isonitrogenous L-alanine, respectively, representing Gin group or control group. Serum samples were collected to characterize metabolites after a 7-d treatment. Results showed that twenty metabolites were down-regulated significantly （P〈0.05） in control piglets compared with suckling ones. These data demonstrated that early weaning causes a wide range of metabolic changes across arginine and proline metabolism, aminosugar and nucleotide metabolism, galactose metabolism, glycerophospholipid metabolism, biosynthesis of unsaturated fatty acid, and fatty acid metabolism. Dietary Gin supplementation increased the levels of creatinine, D-xylose, 2-hydroxybutyric acid, palmitelaidic acid, and a-L-galactofuranose （P〈0.05） in eady weaned piglets, and were involved in the arginine and proline metabolism, carbohydrate metabolism, and fatty acid metabolism. A leave-one-out cross-validation of random forest analysis indicated that creatinine was the most important metabolite among the three groups. Notably, the concentration of creatinine in control piglets was decreased （P=0.00001） compared to the suckling piglets, and increased （P=0.0003） in Gin-supplemented piglets. A correlation network for weaned and suckling piglets revealed that early weaning changed the metabolic pathways, leading to the abnormality of carbohydrate metabolism, amino acid metabolism, and lipid metabolism, which could be partially improved by dietary Gin supplementation. These findings provide fresh insight into the complex metabolic changes in response to early weaning and dietary Gin supplementation in piglets.

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.

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.