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Background Volatile organic compounds (VOCs) in exhaled breath are closely associated with respiratory diseases and are linked to various metabolic reactions in the human body. A quantitative analytical method can provide technical support for studying VOCs related to various diseases. Objective To establish a thermal desorption-gas chromatography-mass spectrometry (TD-GC-MS) method for the determination of 27 VOCs in exhaled breath. Methods VOCs in exhaled breath were collected using a Bio-VOC sampler and enriched with Tenax TA thermal desorption tubes before TD-GC-MS analysis. Standards were collected using thermal desorption tubes and optimized for thermal desorption conditions as well as chromatographic and mass spectrometric conditions: The separation of the 27 VOCs was achieved by an optimized temperature program, the improvement of sensitivity by optimizing quantitative ions, and the increase of VOCs desorption efficiency by optimizing thermal desorption time and temperature. Limit of detection, limit of quantification, accuracy, precision, and stability of the proposed method were investigated by spiking with a blank gas bag, and exhaled breath samples from 20 healthy individuals were collected for an application study of the proposed method. Results The thermal desorption temperature was 280 ℃, and desorption time was 6 min. A VF-624ms chromatographic column was selected for the separation of target substances. The initial temperature of heating program was 35 ℃, maintained for 1 min, and then increased to 100 ℃ at a heating rate of 3 ℃·min−1 for 1 min, followed by increasing to 210 ℃ at a heating rate of 28 ℃·min−1 for 5 min. A quantitative analysis was conducted with a single ion monitoring (SIM) mode. Under these conditions, the 27 VOCs showed good linear relationships in their respective concentration ranges and the correlation coefficients were higher than 0.9990. The limits of detection of the method were in the range of 0.01-0.13 nmol·mol−1, the limits of quantification were in the range of 0.02-0.44 nmol·mol−1, and the spiked recoveries were in the range of 80.1%-120.5%, with intra-batch and inter-batch precision ≤ 18.8% and 17.9% respectively. All substances can be stored at room temperature (23-28 °C) for 7 d and at 4 °C for 14 d. The proposed method was applied to exhaled breath samples from 20 subjects with detection rates≥ 80% (except for trans-2-pentene and decane) and a concentration range of 0.00-465.50 nmol·mol−1. Conclusion The established TD-GC-MS method for quantification of VOCs in exhaled breath is characterized by high sensitivity and good accuracy, and is suitable for quantitative determination of VOCs in exhaled breath, which can provide technical support for the study of exhaled breath VOCs.
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ObjectiveTo screen the differential markers by analyzing volatile components in Dalbergia odorifera and its counterfeits， in order to provide reference for authentication of D. odorifera. MethodThe volatile components in D. odorifera and its counterfeits were detected by headspace gas chromatography-mass spectrometry（HS-GC-MS）， and the GC conditions were heated by procedure（the initial temperature of the column was 50 ℃， the retention time was 1 min， and then the temperature was raised to 300 ℃ at 10 ℃ for 10 min）， the carrier gas was helium， and the flow rate was 1.0 mL·min-1， the split ratio was 10∶1， and the injection volume was 1 mL. The MS conditions used electron bombardment ionization（EI） with the scanning range of m/z 35-550. The compound species were identified by database matching， the relative content of each component was calculated by the peak area normalization method， and principal component analysis（PCA）， orthogonal partial least squares-discrimination analysis（OPLS-DA） and cluster analysis were performed on the detection results by SIMCA 14.1 software， and the differential components of D. odorifera and its counterfeits were screened out according to the variable importance in the projection（VIP） value>2 and P<0.05. ResultA total of 26， 17， 8， 22， 24 and 7 volatile components were identified from D. odorifera， D. bariensis， D. latifolia， D. benthamii， D. pinnata and D. cochinchinensis， respectively. Among them， there were 11 unique volatile components of D. odorifera， 6 unique volatile components of D. bariensis， 3 unique volatile components of D. latifolia， 6 unique volatile components of D. benthamii， 8 unique volatile components of D. pinnata， 4 unique volatile components of D. cochinchinensis. The PCA results showed that， except for D. latifolia and D. cochinchinensis， which could not be clearly distinguished， D. odorifera and other counterfeits could be distributed in a certain area， respectively. The OPLS-DA results showed that D. odorifera and its five counterfeits were clustered into one group each， indicating significant differences in volatile components between D. odorifera and its counterfeits. Finally， a total of 31 differential markers of volatile components between D. odoriferae and its counterfeits were screened. ConclusionHS-GC-MS combined with SIMCA 14.1 software can systematically elucidate the volatile differential components between D. odorifera and its counterfeits， which is suitable for rapid identification of them.
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Objective To establish a rapid qualitative analysis method for volatile organic components in chemicals. Methods Headspace gas chromatography-mass spectrometry was used to qualitatively determine 19 volatile organic components, including benzene, 1,2-dichloroethane, and n-hexane, in chemicals. Different sample amounts, heating temperatures, heating times, and sample volumes were analyzed to assess their effects on detection results and optimize sampling conditions. Results Based on the set chromatography, the optimal sampling process of this method was as follows： 5.0 g sample in a 20.0 mL headspace bottle, incubated at 40 ℃ for 30 minutes in a constant-temperature drying incubator, and a 1.00 mL headspace gas injection. The within-run and between-run relative standard deviations of all components ranged from 0.00% to 21.05% and 0.00% to 33.33%, respectively. The samples stored in sealed glass containers were stable at room temperature for at least 60 days. Conclusion This method offers simplicity, good reproducibility, and stability, making it suitable for rapid qualitative analysis of volatile organic components in chemicals.
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@#[Objective] To explore the application of Quality by Design (QbD) tools in assessing geographical variations of Phyllanthus emblica (P. emblica) from five distinct Indian states. [Methods] In the current experiment, the Box-Behnken design with a reduced quartic model and 105 runs was employed with the use of the Design Expert software for randomized response surface mapping. Three different extraction methods (Soxhlet, maceration, and sonication) along with three solventst [distilled water, methanol, and water-methanol mixture (50 : 50 v/v)] were considered in the present study. The anti-oxidant activities, total flavonoid content (TFC), and total phenolic content (TPC) in the P. emblica were determined and analysed by gas chromatography-mass spectrometry (GC-MS) to identify the major components. [Results] The QbD overlay plot showed that the extractive value of the P. emblica was no less than 30% w/w, 2,2-diphenyl-1-picrylhydrazyl (DPPH) no less than 60% mcg/mL (micrograms per millilitre), TFC no less than 75 mg QE/g (milligrams of quercetin equivalents per gram), and TPC no less than 80 mg GAE/g (milligrams of gallic acid equivalents per gram). Moreover, the GC-MS data confirmed the presence of variation in the bioactives of P. emblica extracts. [Conclusion] The model was significant in describing the variation in extractive value, DPPH, TFC, and TPC. The QbD approach may tend to prioritize thoroughness in the extraction process, ultimately resulting in improved quality in the extracted products.
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ObjectiveBy exploring the volatile components， polysaccharide composition and changes in the contents of five carbohydrate components of Polygonatum cyrtonema rhizoma before and after processing， and then the effect of yellow rice wine on the odour formation of P. cyrtonema rhizoma was investigated. MethodThe volatile components of P. cyrtonema rhizoma before and after processing were detected by headspace gas chromatography-mass spectrometry（HS-GC-MS）， and sample data were subjected to principal component analysis（PCA） and orthogonal partial least squares-discriminant analysis（OPLS-DA） using SIMCA 14.1， then the differences between these components of P. cyrtonema rhizoma before and after processing were screened according to the principle of variable importance in the projection（VIP） value>1. Crude carbohydrate components in raw and wine-processed P. cyrtonema rhizoma were subjected to oxime and silylation， the carbohydrate components were analyzed by gas chromatography-mass spectrometry（GC-MS/MS）， and the relative contents of various components were calculated by peak area normalization， then quantitative analysis of four carbohydrate components was also carried out. ResultA total of 23 volatile components were identified from the raw products and the wine-processed products， including 15 components in raw products and 20 components in wine-processed products. Among them， 2-methylbutyraldehyde and isovaleraldehyde had a sweet odor and their contents increased after processing， but the contents of hexanal and caproic acid decreased， new components such as 2-acetylfuran and 5-methylfuranal were produced after processing. PCA and OPLS-DA results showed that there were significant differences between raw products and the wine-processed products， a total of 13 differential compounds were screened out， of which 7 showed an upward trend in relative content and 6 showed a downward trend. A total of 7 carbohydrate components， including 5 monosaccharides and 2 disaccharides， were identified in raw products and the wine-processed products. The results of determination showed that the contents of fructose， glucose， mannose and sucrose in P. cyrtonema rhizoma increased after wine-processing， and their increases were 4.54， 1.51， 2.93， 3.66 times， respectively. ConclusionAfter processing， the increase of aromatic flavor of P. cyrtonema rhizoma may be related to the increase of the contents of aldehydes such as 2-methylbutyraldehyde and isovaleraldehyde， while the decrease of raw flavor may be related to the decrease of the contents of volatile components such as hexanal and hexanoic acid， the increase of sweet flavor may be related to the increase of the contents of monosaccharides and oligosaccharides such as fructose and sucrose.
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ObjectiveTo investigate the key compounds affecting the irritation and to clarify the effect of heating and the addition of ginger juice as the auxiliary material during the processing on the irritation of Magnoliae Officinalis Cortex（MOC） by comparing the irritation and composition of volatile oil in MOC and its different processed products. MethodVolatile oil in raw products， water-processed products， ginger-dried products， ginger-fried products（the amounts of ginger were 10%， 50%， respectively） of MOC were extracted by steam distillation and subjected to rabbit eye irritation experiment， and the volatile components of each sample were detected by gas chromatography-mass spectrometry（GC-MS）. Principal component analysis（PCA）and orthogonal partial least squares-discriminant analysis（OPLS-DA） were used to analyze the data of each sample by SIMCA 14.1. The relative contents of different processed products were compared two by two with those of and raw products or ginger-fried products， and the markers that might be related to the irritation were sorted out according to the principles of variable importance in the projection（VIP） value >1 and P<0.05， and the factors influencing the differences in irritation were analyzed. ResultCompared with the blank group， the administration groups all had irritation to the eyes of rabbits， and the degree of irritation was in the order of raw products>water-processed products>ginger-dried products>ginger-fried products（10%）>ginger-fried products（50%）. The results of PCA and OPLS-DA showed that there were differences in the volatile oil from raw products and different processed products. According to VIP value>1 and P<0.05， and combined with the results of eye irritation experiment， ten volatile compounds related to irritation changes were screened out. Among them， cis-cinnamaldehyde was only detected in raw products， the relative contents of β-caryophyllene， （+）-delta-cadinene， α-humulene， γ-muurolene， （-）-isoledene and citral all increased to different degrees， the contents of p-cymene， 1（10）-4-cadinadien-15-ol and β-eudesmol all decreased to different degrees. ConclusionThe irritation of MOC is reduced after heating and processing with ginger juice， and the synergistic effect of both is more effective for reducing irritation. Among the differential markers associated with changes in irritation， the increase in the relative content of citral is closely related to the addition of ginger juice， while the decrease in the relative contents of cis-cinnamaldehyde， p-cymene， 1（10）-4-cadinadien-15-ol is related to heating， and the changes of other components may be related to the synergistic effect of heating and ginger juice.
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ObjectiveTo analyze the fingerprint of six pungent herbs based on the molecular connectivity index（MCI）and the matching frequency total statistical moment method， and to study the division and integration of the "imprinting template" of their volatile components， so as to find the common "imprinting template" characteristics of the pungent herbs. MethodThe volatile components of six pungent herbs were extracted by steam distillation， and their fingerprints were established by gas chromatography-mass spectrometry（GC-MS） with a programmed temperature increase（80 ℃ for 5 min， 5 ℃·min-1 to 200 ℃ for 5 min， 2 ℃·min-1 to 230 ℃ for 10 min）， a splitting ratio of 20∶1， an electron bombardment ion source（EI） and the detection range of m/z 35-650， and the average MCI and total statistical moment parameters of the fingerprints were calculated. Then the matching frequency method was used to classify， integrate and confirm the chromatographic peaks of the fingerprints of six pungent herbs. ResultThe average zero order， first-order and second-order MCI values of the volatile components of Pogostemonis Herba， Artemisiae Argyi Folium， Atractylodis Rhizoma， Asari Radix et Rhizoma， Magnoliae Flos and Schizonepetae Herba were 9.02， 5.28 and 5.05， respectively. The average values of peak number， total zero-order moment， total first-order moment and total second-order moment were 60， 169×107， 22.49 min and 36.82 min2， respectively. The 20 integrated imprinting templates were obtained by the matching frequency method for the six pungent herbs， among which three were common imprinting templates with the retention times of （25.97±0.21），（26.90±0.20），（31.64±1.24） min， respectively， and the representative components were valencene，β-elemene， caryophyllin， etc. ConclusionMCI combined the matching frequency total statistical moment can divide and integrate the characteristics of imprinting templates of six pungent herbs， and find their common chromatographic imprinting characteristics， which can provide a reference for the determination of effective substances of pungent herbs.
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ObjectiveBy comparing the differences in composition and content of volatile components between Atractylodis Macrocephalae Rhizoma（AMR）and bleaching AMR， bran-fried AMR and bran-fried bleaching AMR， the effect of processing with rice-washed water on the volatile components in AMR and bran-fried AMR were investigated. MethodHeadspace gas chromatography-mass spectrometry（HS-GC-MS）was used to determine the volatile components in raw products， bran-fried products and their processed products with rice-washed water. GC conditions were programmed temperature（starting temperature of 50 ℃， rising to 140 ℃ at 10 ℃·min-1， maintained for 5 min， then rising to 210 ℃ at 4 ℃·min-1）， splitting ratio of 10∶1， high purity helium as the carrier gas and a solvent delay time of 3 min. MS conditions were an electron bombardment ion source（EI） with an electron collision energy of 70 eV， ion source temperature of 230 ℃， and the detection range of m/z 20-650. The relative contents of the components were determined by the peak area normalization method， the obtained sample data were subjected to principal component analysis（PCA） and orthogonal partial least squares-discriminant analysis（OPLS-DA） by SIMCA 14.1 software， and the differential components of AMR and bleaching AMR， and bran-fried AMR and bran-fried bleaching AMR were screened according to variable importance in the projection（VIP） value>1 and P<0.05. ResultA total of 71 volatile components were identified， including 53 in AMR， 50 in bleaching AMR， 51 in bran-fried AMR， and 44 in bran-fried bleaching AMR. OPLS-DA results showed that there were significant differences between AMR and bleaching AMR， bran-fried AMR and bran-fried bleaching AMR， but not between AMR samples from different origins. The compound composition of AMR and bleaching AMR， bran-fried AMR and bran-fried bleaching AMR did not change， but the contents of monoterpenes and sesquiterpenes changed significantly. ConclusionSignificant changes in the contents of volatile components were observed in AMR and bleaching AMR， bran-fried AMR and bran-fried bleaching AMR， among them， 1，2-dimethyl-4-methylidenecyclopentene， 9，10-dehydro-isolongifolene， γ-elemene， zingiberene， atractylone， silphinene， modhephene and （1S，4S，4aS）-1-isopropyl-4，7-dimethyl-1，2，3，4，4a，5-hexahydronaphthalene can be used as candidate differential markers of volatile components of AMR before and after processing with rice-washed water.
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The menace of drug resistant pathogens is increasing and their level of evading conventional antimicrobials is rising. It is therefore important to discover new antimicrobials to counter the current challenges. Our preliminary investigation identified Bacillus subtilis subsp. subtilis 168 isolated from soil sample sourced from a river bank in Abuja, Nigeria, as the most potent antibiotic-producing bacteria among the other identified producers. The current study screened for the antimicrobial activity of the extract and fractions of the isolate by broth microdilution method. The minimum inhibitory concentration (MIC), minimum bactericidal concentration (MBC) and the ratio of the MBC/MIC were determined. All the tested pathogens were susceptible to the ethyl-acetate extract (MIC between 28.70 mg/ml and 57.40 mg/ml). The extract displayed bactericidal activity against all tested pathogens (MBC/MIC between 1.00 and 2.00) while Proteus mirabilis was least susceptible. The extract was purified by vacuum liquid chromatography and the fractions challenged with pathogenic strains. The fraction E was the most potent (MIC between 0.09 mg/ml and 0.75 mg/ml) and also bactericidal against all the test microbes (MBC/MIC between 2.00 and 2.11). GC-MS analysis of the purified sub fraction obtained from fraction E identified 13 compounds with different Retention time and peak areas. Among these were three major compounds which include: (i) bis(2-ethylhexyl) phthalate (ii) 1,4-epoxynaphthalene-1(2H)-methanol, 4,5,7-tris(1,1-dimethylethyl)-3,4-dihydro- (iii) D:B-Friedo-B':A'-neogammacer-5-en-3-ol, (3.beta.)-. Our findings suggest that Bacillus subtilis subsp. subtilis 168 isolated locally could serve as a valuable source of lead compounds for pharmaceutical and biotechnological purposes.
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Mesmo reduzida e fragmentada, o vasto bioma da Mata Atlântica abriga milhares de plantas. Como destaque, tem-se as espécies frutíferas, aos quais podem ser atribuídas um importante valor para a segurança alimentar, nutricional e sociocultural. Entre elas, têm-se a cereja-do-rio grande (Eugenia involucrata DC.) e a grumixama (Eugenia brasiliensis Lam.), caracterizadas pela polpa de sabor doce-acidulado, sendo muito apreciadas e utilizadas tanto in natura, quanto no preparo de doces, xaropes, licores e geleias. Uma das características determinantes para o sucesso e aceitação destes frutos pelo consumidor, são os atributos de qualidade sensorial. As propriedades aromáticas dos frutos dependem da potência individual dos voláteis e a concentração de cada um, bem como a combinação com outros compostos. Todavia, apesar do grande potencial de mercado, devido às características nutricionais, fitoterápicas, potencial funcional e ao sabor exótico, os plantios existentes destas são oriundos de multiplicação por sementes, resultando em plantas desuniformes quanto as características de produção e qualidade. Neste sentido, o presente trabalho teve como objetivo identificar metabólitos voláteis que confiram características sensoriais desejáveis aos frutos. Auxiliando na identificação de plantas que produzem frutos com voláteis de interesse para o sabor, o que permitirá a clonagem e propagação de plantas com homogeneidade na produção. Os compostos voláteis foram analisados em triplicata, de acordo com o método de microextração em fase sólida (SPME, do inglês Solid Phase Microextraction). Os resultados mostraram que os grupos de frutos das diversas regiões se diferenciaram quanto a composição dos metabolitos voláteis, bem como na abundância destes compostos. Observou-se também uma variação de composição entre as árvores da mesma região demonstrando tal irregularidade ocasionada pela propagação por sementes. A maioria de compostos voláteis produzidos foram identificados como terpenos, sendo estes já conhecidos pela importância no flavor em frutos. Desta forma, conhecer o aroma fornecerá um conjunto de dados que são subsídios para outros pesquisadores trabalharem em suas diversas áreas buscando características necessárias para o sucesso da comercialização, ocasionando no incentivo ao cultivo e valorização da riqueza nacional, no âmbito das espécies frutíferas, com vistas à proteção ambiental e em defesa da biodiversidade brasileira
The Atlantic Forest harbors thousands of plants despite of its reduced and fragmented character. It is important to highlight the fruit species which hold attributed and important value for food and socio-cultural security. Among them, there are the big cherry (Eugenia involucrata DC.) And the grumixama (Eugenia brasiliensis Lam.), fruit with sweet-acidulated flavor, which is much appreciated and used in the preparation of sweets, syrups, liqueurs, and jellies. One of the determining characteristics for the success and acceptance of these fruits by the consumer are the attributes of sensorial quality. The aromatic properties of the fruits depend on the individual potency of the volatiles and the concentration in each one of them, as well as the combination with other compounds. Despite of the great market potential due to the nutritional, phytotherapic and exotic flavor characteristics, the existing plantations of these fruits are originated from seed multiplication, resulting on uneven plants in terms of production and quality characteristics. In this sense, the presented work below was aimed to identify volatile metabolites that confer desirable sensorial characteristics to the fruits. The volatile compounds were analyzed in triplicate according to the Solid Phase Microextraction (SPME) method. The results showed that the fruit groups from different regions differed in terms of the composition of volatile metabolites, as well as in the abundance of these compounds. There was also a variation of composition among the trees of the same region which demonstrated such heterogeneity caused by seed propagation. Most volatile compounds produced were identified as terpenes which are known for playing an important role in the flavor of fruits. In this way, by knowing the aroma, a set of data will be provided and used as an allowance for other researchers who are working in the various areas related to the pursue of the necessary characteristics for the commercial success, resulting on the motivation to cultivate and value the forest
Subject(s)
Myrtaceae/classification , Volatile Organic Compounds/adverse effects , Eugenia , Fruit/classification , Plants , World Health Organization , Conservation of Natural Resources/methods , Biodiversity , Gas Chromatography-Mass Spectrometry/methods , OdorantsABSTRACT
Mesmo reduzida e fragmentada, o vasto bioma da Mata Atlântica abriga milhares de plantas. Como destaque, tem-se as espécies frutíferas, aos quais podem ser atribuídas um importante valor para a segurança alimentar, nutricional e sociocultural. Entre elas, têm-se a cereja-do-rio grande (Eugenia involucrata DC.) e a grumixama (Eugenia brasiliensis Lam.), caracterizadas pela polpa de sabor doce-acidulado, sendo muito apreciadas e utilizadas tanto in natura, quanto no preparo de doces, xaropes, licores e geleias. Uma das características determinantes para o sucesso e aceitação destes frutos pelo consumidor, são os atributos de qualidade sensorial. As propriedades aromáticas dos frutos dependem da potência individual dos voláteis e a concentração de cada um, bem como a combinação com outros compostos. Todavia, apesar do grande potencial de mercado, devido às características nutricionais, fitoterápicas, potencial funcional e ao sabor exótico, os plantios existentes destas são oriundos de multiplicação por sementes, resultando em plantas desuniformes quanto as características de produção e qualidade. Neste sentido, o presente trabalho teve como objetivo identificar metabólitos voláteis que confiram características sensoriais desejáveis aos frutos. Auxiliando na identificação de plantas que produzem frutos com voláteis de interesse para o sabor, o que permitirá a clonagem e propagação de plantas com homogeneidade na produção. Os compostos voláteis foram analisados em triplicata, de acordo com o método de microextração em fase sólida (SPME, do inglês Solid Phase Microextraction). Os resultados mostraram que os grupos de frutos das diversas regiões se diferenciaram quanto a composição dos metabolitos voláteis, bem como na abundância destes compostos. Observou-se também uma variação de composição entre as árvores da mesma região demonstrando tal irregularidade ocasionada pela propagação por sementes. A maioria de compostos voláteis produzidos foram identificados como terpenos, sendo estes já conhecidos pela importância no flavor em frutos. Desta forma, conhecer o aroma fornecerá um conjunto de dados que são subsídios para outros pesquisadores trabalharem em suas diversas áreas buscando características necessárias para o sucesso da comercialização, ocasionando no incentivo ao cultivo e valorização da riqueza nacional, no âmbito das espécies frutíferas, com vistas à proteção ambiental e em defesa da biodiversidade brasileira
The Atlantic Forest harbors thousands of plants despite of its reduced and fragmented character. It is important to highlight the fruit species which hold attributed and important value for food and socio-cultural security. Among them, there are the big cherry (Eugenia involucrata DC.) And the grumixama (Eugenia brasiliensis Lam.), fruit with sweet-acidulated flavor, which is much appreciated and used in the preparation of sweets, syrups, liqueurs, and jellies. One of the determining characteristics for the success and acceptance of these fruits by the consumer are the attributes of sensorial quality. The aromatic properties of the fruits depend on the individual potency of the volatiles and the concentration in each one of them, as well as the combination with other compounds. Despite of the great market potential due to the nutritional, phytotherapic and exotic flavor characteristics, the existing plantations of these fruits are originated from seed multiplication, resulting on uneven plants in terms of production and quality characteristics. In this sense, the presented work below was aimed to identify volatile metabolites that confer desirable sensorial characteristics to the fruits. The volatile compounds were analyzed in triplicate according to the Solid Phase Microextraction (SPME) method. The results showed that the fruit groups from different regions differed in terms of the composition of volatile metabolites, as well as in the abundance of these compounds. There was also a variation of composition among the trees of the same region which demonstrated such heterogeneity caused by seed propagation. Most volatile compounds produced were identified as terpenes which are known for playing an important role in the flavor of fruits. In this way, by knowing the aroma, a set of data will be provided and used as an allowance for other researchers who are working in the various areas related to the pursue of the necessary characteristics for the commercial success, resulting on the motivation to cultivate and value the forest
Subject(s)
Myrtaceae/anatomy & histology , Volatile Organic Compounds , Eugenia/anatomy & histology , Fruit/adverse effects , Plants/adverse effects , Solid Phase Microextraction/methods , Gas Chromatography-Mass Spectrometry/methods , Odorants/analysisABSTRACT
OBJECTIVES@#To establish a combined high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) and gas chromatography-mass spectrometry (GC-MS) method to detect the synthetic cannabinoid CUMYL-PEGACLONE in e-cigarette oil and hair.@*METHODS@#HPLC-MS/MS and GC-MS were used to establish the detection method of CUMYL-PEGACLONE, and the hair of drug-involved persons and the seized e-cigarette oil were detected.@*RESULTS@#The main mass spectrometry characteristic ions m/z of CUMYL-PEGACLONE measured by GC-MS were 91, 179, 197, 254 and 372. CUMYL-PEGACLONE had a good linear relationship in the mass concentration range of 2-50 ng/mL, and the linear correlation coefficient (r) was greater than 0.99. The limit of detection (LOD) of CUMYL-PEGACLONE in hair was 0.01 ng/mg, and the limit of quantitation (LOQ) was 0.02 ng/mg. The LOD of CUMYL-PEGACLONE in e-cigarette oil was 1 ng/mg, and the LOQ was 2 ng/mg. The average recoveries of CUMYL-PEGACLONE under the attempt at high, intermediate and low levels in blank human hair and e-cigarette oil matrix were 98.2%-132.4% and 93.5%-110.6%, and the intraday and intraday precision were 1.2%-12.9% and 0.7%-2.9%. CUMYL-PEGACLONE was detected in the hair of 15 drug-involved persons. Except for 1 person who was lower than LOQ, the concentration of CUMYL-PEGACLONE in the hair of other 14 persons was 0.035-0.563 ng/mg. The mass fraction of CUMYL-PEGACLONE in 2 e-cigarette oil were 0.17% and 0.21%, respectively.@*CONCLUSIONS@#The established HPLC-MS/MS and GC-MS methods are applied to the detection of HPLC-MS/MS in drug-related cases, which provides strong evidence support for the handling authority to quickly investigate these cases, and also provides a reference for the identification of such substances in future.
Subject(s)
Humans , Illicit Drugs/analysis , Tandem Mass Spectrometry , Electronic Nicotine Delivery Systems , Cannabinoids , Hair/chemistry , Limit of Detection , Substance Abuse Detection/methodsABSTRACT
ObjectiveBy comparing the difference of volatile components of the decoction pieces before and after being processed by braising method of Jianchangbang and steaming method included in the 2020 edition of Chinese Pharmacopoeia， the influence of processing methods on the flavor formation of Polygoni Multiflori Radix （PMR） was compared. MethodHeadspace-gas chromatography-mass spectrometry （HS-GC-MS） was used to detect the volatile components of 30 batches of PMR samples from 3 origins with 3 processing methods. The GC was performed under programmed temperature （starting temperature of 40 ℃， rising to 150 ℃ at 5 ℃·min-1， and then rising to 195 ℃ at 10 ℃·min-1） with high purity helium as carrier gas and the split ratio of 10∶1. Mass spectrometry conditions were electron impact ion source （EI） and the detection range of m/z 50-650， the peak area normalization method was used to calculate the relative mass fraction of each component. The chromaticity values of different processed products were measured by a precision colorimeter， the relationship between chromaticity values and relative contents of volatile components was investigated by OriginPro 2021， principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis （OPLS-DA） were performed on the sample data by SIMCA14.1. The differential components of different processed products of PMR were screened according to the principle of variable importance in the projection （VIP） value>1.5， and the material basis of different odor formation of PMR and its processed products was explored. ResultA total of 59 volatile components were identified， among which 34 were raw products， 33 were braised products， and 27 were steamed products. PCA and OPLS-DA results showed that there were significant differences between the three， but there was no significant difference between samples from different origins of the same processing method. Color parameters of a*， b*， E*ab had no significant correlation with contents of volatile components， while L* was negatively correlated with contents of 2-methyl-2-butenal， 2-methyltetrahydrofuran-3-one and 2，3-dihydro-3，5-dihydroxy-6-methyl-4（H）-pyran-4-one （P<0.05）. The contents of pungent odor components such as caproic acid， nonanoic acid and synthetic camphor decreased after processing， while the contents of sweet flavor components such as 2-methyl-2-butenal， furfural and 5-hydroxymethylfurfural increased after processing， and the contents of furfural， 5-methyl-2-furanmethanol， 5-hydroxymethylfurfural and other aroma components in the braised products were significantly higher than that in the steamed products. ConclusionHS-GC-MS can quickly identify the volatile substance basis that causes the different odors of PMR and its processed products. The effect of processing methods on the odor is greater than that of origin. There is a significant correlation between the color parameter of L* and contents of volatile components， the "raw" taste of PMR may be related to volatile components such as caproic acid， pelargonic acid and synthetic camphor， the "flavor" after processing may be related to the increase of the contents of 2-methyl-2-butenal， furfural， 5-hydroxymethylfurfural， methyl maltol and furfuryl alcohol.
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ObjectiveOn the basis of sensory evaluation， the changes of volatile components in gecko before and after processing were compared， and the odor correction effect of different processing methods of gecko was discussed. MethodRaw products， fried yellow products， vinegar processed products， wine processed products， talcum powder scalding products and white wine sprayed products after scalding talcum powder of gecko were prepared， and 10 odor assessors were invited to evaluate the 6 samples in turn by sensory evaluation. Headspace solid-phase microextraction-gas chromatography-mass spectrometry （HS-SPME-GC-MS） and relative odor activity value （ROAV） were used to analyze the key odor components， and multivariate statistical methods were used to analyze the difference of volatile components between raw and processed products of gecko. Taking water-soluble extract and protein contents as internal indicators， sensory evaluation score and content ranking of differential components as external indicators， and assigning a weight of 0.25 to them respectively， the comprehensive scores of raw products and processed products of gecko were calculated to evaluate the odor correction effect of each processing method. ResultThe average sensory evaluation scores of the raw products， fried yellow products， vinegar processed products， wine processed products， talcum powder scalding products and white wine sprayed products after scalding talcum powder of gecko were 1.6， 5.2， 6.2， 6.1， 7.2 and 8.0， respectively. ROAV results showed that key components affecting odor of gecko were 2-ethyl-3，5-dimethylpyrazine， isovaleraldehyde， trimethylamine， 1-octen-3-ol， n-octanal， nonanal， 2-methylnaphthalene， γ-octanolide， 2-heptanone and phenol. Principal component analysis （PCA） significantly distinguished raw products from processed products. Orthogonal partial least squares-discriminant analysis （OPLS-DA） results showed that there were 16， 13， 16， 16， 16 differential components between raw products， fried yellow products， vinegar processed products， wine processed products， talcum powder scalding products and white wine sprayed products after scalding talcum powder of gecko. Among these differential components， there were 4 common components， namely， the contents of different odor components （2-methylnaphthalene and 2-ethyl-p-xylene） decreased， while the contents of different flavor components （2-decanone and 2，3，5-trimethylpyrazine） increased. The comprehensive scoring results showed that the odor correction effect of each processed products was in the order of talcum powder scalding products>wine processed products>vinegar processed products>fried yellow products>white wine sprayed products after scalding talcum powder. ConclusionTalcum powder scalding is a better method to improve the odor of gecko， and it can provide an experimental basis for the processing of gecko to correct the odor.
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ObjectiveTo study the composition of volatile oil in Opisthopappus taihangensis （Taihangju）， and provide a reference for comprehensive development of this medicine. MethodTaking Chrysanthemum morifolium （Xiaobaiju）， C. morifolium （Xiaohuangju） and C. indicum （Yejuhua） as control， the qualitative and quantitative analysis of volatile oil in Taihangju and three control varieties were completed by gas chromatography-mass spectrometry （GC-MS） combined with retention index method. The GC conditions were as following：programmed temperature （initial temperature at 60 ℃， kept for 2 min； up to 120 ℃ with the heating rate of 5 ℃·min-1， still kept for 2 min； up to 180 ℃ with the heating rate of 2 ℃·min-1， kept for 3 min； and then up to 240 ℃ with the heating rate of 8 ℃·min-1， kept for 5 min； finally up to 280 ℃ with the heating rate of 10 ℃·min-1， kept it for 5 min and finished）， high-purity helium as the carrier gas， the split ratio of 50∶1. MS conditions were as follows：electron impact ion source （EI）， ion source temperature of 230 ℃， electron collision energy of 70 eV and scanning range of m/z 30-445. Principal component analysis （PCA） and orthogonal partial least squares-discriminant analysis （OPLS-DA） were used to obtain the characteristic components between Taihangju and the three control varieties. ResultA total of 86， 96， 112 and 109 compounds including 73 common components were identified in Taihangju， Xiaobaiju， Xiaohuangju and Yejuhua， respectively. The contents of volatile components in Taihangju were significantly different from that of the control varieties. In which， the relative contents of α-thujone， eucalyptol and terpinen-4-ol were high in Taihangju， and eucalyptol， camphor and α-terpinyl acetate were the main compositions in the control varieties. In addition， 11 compounds were screened as characteristic components to distinguish Taihangju and the three control varieties by PCA and OPLS-DA， including main differential components of chamazulene and δ-cadinene. ConclusionThe main components of volatile oil in Taihangju includes alcohols， terpenes， ketones and esters with high medicinal value. The accuracy of qualitative analysis of volatile oil is improved by GC-MS combined with retention index method， which provides scientific reference for development and utilization of Taihangju.
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ObjectiveTaking Chuanxiong Chatiaosan prescription as the carrier， by comparing the differences of volatile components in Chuanxiong Rhizoma with single decoction pieces and compatible prescription of different decoction pieces， the differences of material basic connotation of different formulations of Chuanxiong Chatiaosan were revealed from the aspects of processing （raw and wine-processed products）， compound compatibility and dosage form （powder and decoction）. MethodThe volatile oil was extracted from different decoction pieces of Chuanxiong Rhizoma， Chuanxiong Chatiaosan and its decoction with different decoction pieces of Chuanxiong Rhizoma by steam distillation， the main components and their relative contents were identified by gas chromatography-mass spectrometry （GC-MS）. ResultA total of 25 volatile components were identified from different processed products of Chuanxiong Rhizoma， including 11 monoterpenoids， 4 phenols， 3 sesquiterpenoids， 3 phthalides， 2 ketones and 2 olefins， the contents of α-pinene， β-pinene， 3-butylphthalide and others increased after the raw products was processed with wine. A total of 85 constituents were identified from Chuanxiong Chatiaosan with different decoction pieces， including 31 monoterpenoids， 23 sesquiterpenoids， 5 alcohols， 5 aldehydes， 4 phenols， 4 phthalides， 3 ethers， 3 ketones， 1 olefin， 1 organic acid， 2 esters and 3 other compounds. A total of 22 components， including 9 sesquiterpenoids， 3 phthalides， 2 phenols， 6 monoterpenoids， 1 aldehyde and 1 alkane， were identified from the decoction of Chuanxiong Chatiaosan with different processed products. ConclusionThere was no significant difference in the composition between raw products and wine-processed products of Chuanxiong Rhizoma either in single decoction pieces or in compatibility prescription， but the relative content changed to some extent， and the wine-processed products was the most obvious. There was a great difference in the composition of volatile components between the Chuanxiong Chatiaosan and its decoction. The volatile components， such as isopulegol， isocalamendiol and safrole， were not found in the decoction. Components in Chuanxiong Rhizoma processed with wine will change with the addition of yellow rice wine， and volatile components can reflect the difference between decoction pieces and prescriptions of the wine-processed products.
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ObjectiveTo investigate the metabolites and gene expression characteristics in fibrous roots of Dioscorea zingiberensis in response to low phosphorus stress. MethodThe severe stress group， the moderate stress group， and the normal group were set up to stimulate the low phosphorus stress experiment. The fibrous roots of D. zingiberensis were collected during initial stress. The metabolites and transcriptomic characteristics were analyzed by gas chromatography-mass spectrometry （GC-MS） derivatization and RNA-seq techniques. Through multivariate statistical analysis of metabolites treated by different methods，functional analysis of differentially expressed genes， and data mining， the metabolism markers produced in fibrous roots of D. zingiberensis under low phosphorus stress were screened out， and the metabolic pathway characteristics of different genes were analyzed. ResultA total of 116 GC-MS metabolites were detected from the fibrous roots of D. zingiberensis. The metabolic characteristics of fibrous roots of D. zingiberensis under different low phosphorus treatments were obviously different. Orthogonal partial least squares discriminant analysis（OPLS-DA） model was used to screen six differential metabolites represented by sugars and alcohols from metabolites of fibrous roots treated with different methods，and these components were presumedly metabolism markers of fibrous roots of D. zingiberensis in response to low phosphorus stress. The differential genes screened out from the severe stress group and the normal group were mainly enriched in peroxidase pathway，phosphate and hypophosphate metabolism pathway，while the differential genes screened out from the severe stress group and the moderate stress group were mainly enriched in glutathione metabolism pathway and phosphopentose pathway. A total of 177 differential genes in response to low phosphorus stress were screened out from fibrous roots， involving many pathways such as terpenoid skeleton and inositol biosynthesis，which was consistent with the fact that the metabolic differential components in fibrous roots in response to low phosphorus stress were mainly saccharides and inositol. ConclusionThe metabolites and gene expression in fibrous roots of D. zingiberensis responded to low phosphorus stress，and the differential metabolites were closely related to differentially expressed genes. This study is expected to provide a theoretical basis for the research on the molecular mechanism of D. zingiberensis in response to low phosphorus stress.
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Covalent organic nanospheres(CONs)were explored as a fiber coating for solid-phase microextraction of genotoxic impurities(GTIs)from active ingredients(AIs).CONs were synthesized by an easy solution-phase procedure at 25℃.The obtained nanospheres exhibited a high specific surface area,good ther-mostability,high acid and alkali resistance,and favorable crystallinity and porosity.Two types of GTIs,alkyl halides(1-iodooctane,1-chlorobenzene,1-bromododecane,1,2-dichlorobenzene,1-bromooctane,1-chlorohexane,and 1,8-dibromooctane)and sulfonate esters(methyl p-toluenesulfonate and ethyl p-toluenesulfonate),were chosen as target molecules for assessing the performance of the coating.The prepared coating achieved high enhancement factors(5097-9799)for the selected GTIs.The strong affinity between CONs and GTIs was tentatively attributed to T-T and hydrophobicity interactions,large surface area of the CONs,and size-matching of the materials.Combined with gas chromatography-mass spectrometry(GC-MS),the established analytical method detected the GTIs in capecitabine and imatinib mesylate samples over a wide linear range(0.2-200 ng/g)with a low detection limit(0.04-2.0 ng/g),satisfactory recovery(80.03％-109.5％),and high repeatability(6.20％-14.8％)and reproducibility(6.20％-14.1％).Therefore,the CON-coated fibers are promising alternatives for the sensitive detection of GTIs in AI samples.
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Objective:To analyze the serum and urinary amino acid (AA) profiles of urolithiasis patients to explore the potential biomarkers for clinical screening and early diagnosis.Methods:Case-control study. Serum and urine samples were collected from 74 urolithiasis patients (aged 20-82 years, 41 men, 33 female) in the department of urology of the First Affiliated Hospital of Fujian Medical University and 35 healthy controls (HC, aged 22-80 years old, 20 men, 15 female) from the health examination center from February 2015 to October 2017. Serum and urinary AA levels of patients and HC were analyzed using Gas Chromatography-Mass Spectrometry (GC-MS) based metabolomic strategy. The multivariate statistical analysis methods of principal component analysis (PCA) and orthogonal partial least squares discrimination analysis (OPLS-DA) were employed for modeling. The variable importance projection (VIP) value of OPLS-DA model>1 and P<0.05 of t test were selected to screen the differential amino acid metabolites. The diagnostic capabilities of potential markers were evaluated by receiver operating characteristic (ROC) curve and binary logistic regression analysis. Results:Five AA metabolites including serine, glutamate, aspartic acid, isoleucine and glycine were found, which had statistically significant differences between the patient group and the control group ( P<0.05) and were associated with seven metabolic pathways. Serum serine, glutamate, aspartic acid, isoleucine and urine glycine and aspartic acid were combined into an integrated marker panel whose AUC value was 0.890, the sensitivity was 78.0%, and the specificity was 96.4%. Conclusion:Five amino acids in serum and urine could be used as an integrated biomarker panel for the clinical screening and early diagnosis of urolithiasis, which could provide some experimental basis for molecular urolithiasis research.
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Docosanol is the only US Food and Drug Administration(FDA)approved over-the-counter topical product for treating recurrent oral-facial herpes simplex labialis.Validated analytical methods for docosanol are required to demonstrate the bioequivalence of docosanol topical products.A gas chromatography/selected ion monitoring mode mass spectrometry(GC/SIM-MS)method was developed and validated for docosanol determination in biological samples.Docosanol and isopropyl palmitate(internal standard)were separated on a high-polarity GC capillary column with(88％cyanopropy)aryl-polysiloxane employed as the stationary phase.The ions of m/z 83 and 256 were selected to monitor docosanol and isopropyl palmitate,respectively;the total run time was 20 min.The GC/SIM-MS method was validated in accordance with US FDA guidelines,and the results met the US FDA acceptance criteria.The docosanol calibration standards were linear in the 100-10000 ng/mL concentration range(R2＞0.994).The recoveries for docosanol from the receptor fluid and skin homogenates were＞93.2％and＞95.8％,respectively.The validated method was successfully applied to analyze ex vivo human cadaver skin permeation samples.On applying Abreva?cream tube and Abreva?cream pump,the amount of doco-sanol that penetrated human cadaver skin at 48 h was 21.5±7.01 and 24.0±6.95 ng/mg,respectively.Accordingly,we concluded that the validated GC/SIM-MS was sensitive,specific,and suitable for quantifying docosanol as a quality control tool.This method can be used for routine analysis as a cost-effective alternative to other techniques.