Comparison on Changes of Volatile Components in Gecko Before and After Processing by HS-SPME-GC-MS / 中国实验方剂学杂志

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.

Analysis of Quality Changes of Platycladi Semen Before and After Deterioration Based on HS-SPME/GC-MS and Electronic Sensory Technology / 中国实验方剂学杂志

ObjectiveTo analyze the quality changes of Platycladi Semen before and after the deterioration of moth-eaten and rancidity during storage. MethodFour types samples of Platycladi Semen， including normal， moth-eaten， oxidative rancidity and hydrolytic rancidity， were determined for volatile components， odor， and taste based on headspace solid phase microextraction/gas chromatography-mass spectrometry （HS-SPME/GC-MS） and electronic sensory techniques such as electronic nose and electronic tongue. Volatile components were identified by searching the database and manual comparison， the odor and taste were determined by the response values of the electronic nose and electronic tongue sensors， and the difference between samples before and after deterioration was studied by multivariate statistical analysis. ResultA total of 85 compounds were identified in Platycladi Semen samples. Compared with the normal samples， the number of volatile compounds in samples after hydrolytic rancidity decreased by 5， the number of volatile compounds in samples after moth-eaten and oxidative rancidity increased by 1 and 21， respectively. Aldehydes and acids accounted for majority of types. Among them， the contents of N-hexanoic acid， hexanal and propionic acid in the samples of oxidative rancidity reached 11.49%， 10.21% and 7.52%， which became the key indicators of rancidity. There was significant variance among the odor components corresponding to W1W， W2W and W1S sensors by electronic nose analysis. It was indicated that the value of sourness in deteriorated samples generally increased by mean of electronic tongue analysis. Compared with normal samples， the moth-eaten samples had changed slightly and rancidity samples had changed significantly especially oxidative rancidity samples of volatile components， odor and taste by multivariate statistical analysis. ConclusionIn terms of Platycladi Semen， the oxidative rancidity caused by nature storage for 12 months has the greatest impact on the quality. Therefore， it should be mainly to prevent oxidative rancidity to ensure the quality of Platycladi Semen.

Induced volatiles in the interaction between soybean (Glycine max) and the Mexican soybean weevil (Rhyssomatus nigerrimus) / Voláteis induzidos na interação entre soja (Glycine max) e gorgulho da soja mexicana (Rhyssomatus nigerrimus)

Abstract The present study analyzed the volatile compounds emitted by Glycine max (cv. FT-Cristalina-RCH) soybean plants: healthy plants and plants damaged mechanically or by the Mexican soybean weevil Rhyssomatus nigerrimus. The SPME method was used to compare the volatile profile of soybean plants in four different conditions. The volatile profile of G. max plants infested by R. nigerrimus was qualitatively and quantitatively different from that of healthy and mechanically damaged plants. Emission of 59 compounds was detected in the four treatments. Of these compounds, 19 were identified by comparison of the Kovats index, mass spectrum and retention times with those of synthetic standards. An increase in concentration of the volatiles (Z)-3-hexenyl acetate and the compound 1-octen-3-ol was observed when the soybean plants were mechanically damaged. The compounds mostly produced by the soybean plant during infestation by male and female R. nigerrimus were 1-octen-3-ol, 6-methyl-5-hepten-2-one, (E)-β-ocimene, salicylaldehyde, unknown 10, linalool, methyl salicylate, (Z)-8-dodecenyl acetate (ester 5), ketone 2 and geranyl acetone. Behavioral effects of the identified compounds during the insect-plant interaction and their conspecifics are discussed.

Resumo O presente estudo analisou os compostos voláteis emitidos pelas plantas de soja Glycine max (cv. FT-Cristalina-RCH): plantas e plantas sadias danificadas mecanicamente ou pelo gorgulho da soja mexicana Rhyssomatus nigerrimus. O método SPME foi utilizado para comparar o perfil volátil de plantas de soja em quatro diferentes condições. O perfil volátil das plantas de G. max infestadas por R. nigerrimus foi qualitativa e quantitativamente diferente do das plantas saudáveis e danificadas mecanicamente. Foi detectada, nos quatro tratamentos, emissão de 59 compostos, dos quais 19 foram identificados por comparação do índice de Kovats, espectro de massa e tempos de retenção com aqueles de padrões sintéticos. Um aumento na concentração dos voláteis acetato de (Z)-3-hexil e do composto 1-octeno-3-ol foi observado quando as plantas de soja foram mecanicamente danificadas. Os compostos produzidos principalmente pela planta de soja durante a infestação por R. nigerrimus macho e fêmea foram 1-octeno-3-ol, 6-metil-5-hepteno-2-ona, (E)-β-ocimeno, salicilaldeído, desconhecido 10, linalol, salicilato de metila, acetato de (Z)-8-dodecenila (éster 5), cetona 2 e geranil acetona. Foram discutidos os efeitos comportamentais dos compostos identificados durante a interação inseto-planta e seus coespecíficos.

Composição volátil das uvas ao espumante da cv. Chardonnay em diferentes condições de manejo no sul de Minas Gerais (Brasil) / Volatile composition from grapes to sparkling wine of Chardonnay vine in different management conditions in southern of Minas Gerais (Brazil)

O aroma é um dos fatores mais importantes na determinação da qualidade e do caráter do vinho. Isso se deve à presença de compostos voláteis que estão associados às suas características organolépticas ou diferentes proporções entre estes compostos que podem ser influenciadas por fatores vitícolas (clima, solo, cultivar, manejo) e enológicos (maturação da uva, fermentação, tratamentos pósfermentativos). A região do sul de Minas Gerais vem se destacando na produção de espumantes de qualidade, e, nesse contexto, o presente trabalho teve como objetivo conhecer a influência do manejo da videira no desenvolvimento do aroma, da baga até o espumante, a fim de estabelecer associações com a qualidade do produto final. Os experimentos foram realizados com a cultivar Chardonnay em diferentes condições de manejo, em que foram avaliados clones, porta-enxertos, sistemas de condução e densidades de plantio. Foram analisados os compostos voláteis livres por HS-SPME/GC-MS das bagas, mostos, vinhos base e espumantes nas safras 2016, 2017 e 2018. O trabalho foi dividido em quatro partes para a apresentação dos resultados. A primeira consistiu em verificar a influência do material genético na composição volátil da cv. Chardonnay com os experimentos de clones e portaenxertos; a segunda parte avaliou a composição volátil do clone 809 até o espumante; a terceira, em analisar as vinificações dos diferentes sistemas de condução; e a quarta, em avaliar a evolução dos compostos voláteis da baga ao espumante e analisar os aromas que as densidades de plantio podem conferir ao espumante. As principais classes de compostos aromáticos identificados nas matrizes foram: C6-C9 aldeídos, álcoois superiores, aldeídos ramificados, benzenoides, monoterpenoides, norisoprenoides, sesquiterpenoides, cetonas e ácidos graxos. Os resultados mostraram que os clones e os porta-enxertos apresentaram perfis voláteis diferentes, indicando que a variabilidade entre os clones e que a enxertia têm influência no metabolismo da baga; o clone 809 apresenta maior abundância de compostos monoterpenoides, confirmando o seu caráter moscato, das uvas aos espumantes; os diferentes sistemas de condução e densidades de plantio alteram o metabolismo da14 baga, refletindo no perfil volátil dos espumantes nas safras estudadas. Dessa forma, os dados indicam que a composição volátil sofre influência do manejo da videira ao espumante

Aroma is one of the most important factors in determining the quality and character of wine. This is due to the presence of volatile compounds that are associated with their organoleptic characteristics or different proportions among these compounds that can be influenced by viticultural (climate, soil, cultivar, management) and oenological factors (grape maturation, fermentation, post fermentation treatments). The southern region of Minas Gerais has been standing out in the production of quality sparkling wines, and in this context, the purpose of the present work was to learn about the influence of grapevine management on the development of aroma, from berry to sparkling wine, in order to establish associations with the quality of the final product. The experiments were carried out with the Chardonnay cultivar under different management conditions, in which clones, rootstocks, trellising systems and planting densities were evaluated. The free volatile compounds by HS-SPME/GC-MS of the berries, musts, base and sparkling wines in the 2016, 2017 and 2018 harvests were analyzed. The work was divided into four parts in order to present the results. The first part consisted of verifying the influence of genetic material on the volatile composition of the cv. Chardonnay with the experiments on clones and rootstocks; the second part evaluated the volatile composition of clone 809 up to the sparkling wine; the third one part analyzed the vinification of the different trainig systems; and the fourth part evaluated the evolution of the volatile compounds from the berry to the sparkling wine and analyzed the aromas that the planting densities can confer to the sparkling wine. The main classes of aromatic compounds identified in the matrices were: C6-C9 aldehydes, higher alcohols, branched aldehydes, benzenoids, monoterpenoids, norisoprenoids, sesquiterpenoids, ketones and fatty acids. The results showed that the clones and the rootstocks have different volatile profiles, indicating that variability among clones and that grafting have great relevance to the berry secondary metabolism; the 809 clone presents a greater abundance of monoterpenoid compounds, confirming its muscat character, from grapes to sparkling wines; the different training systems and planting densities alter the berry´s metabolism, reflecting16 in the volatile profile of sparkling wines in the studied harvests. The data indicate that the volatile composition is influenced by the management of the berry to the sparkling wine

Establishment and Application of Identification Method for Fishy Odor of Cordyceps Based on HS-SPME/GC-QQQ-MS/MS / 中国实验方剂学杂志

Objective:To establish and apply a new practical analytical method for identifying the fishy odor of Cordyceps based on headspace-solid phase microextraction-gas chromatography-triple quadrupole mass spectrometry （HS-SPME/GC-QQQ-MS/MS） technique. Method:The InertCap Pure-WAX capillary column （0.25 mm×30 m， 0.25 μm） was used for chromatographic separation. The injection port temperature was set at 250 ℃. The injection mode was split injection with a ratio of 5∶1. High purity helium was used as the carrier gas and control mode was set to constant pressure. The column flow rate was 1.43 mL∙min^-1， the linear velocity was 43.3 cm∙s^-1， and the purge flow rate was 3.0 mL∙min^-1. The chromatographic column temperature program as follows：maintained the initial temperature at 50 ℃ for 5 min， and increased the temperature at a rate of 10 ℃∙min^-1 to 250 ℃， held for 10 min. The column equilibrium time was 2.0 min. The ion source of mass spectrographic analysis was electron ionization with ion source temperature of 200 ℃， and the monitoring mode was set to multiple reaction monitoring. Result:Seven batches of Cordyceps samples were collected， including 3 batches from Sichuan， 3 batches from Qinghai and 1 batch from Tibet. There were six batches of counterfeits， including 3 batches from Sichuan， 2 batches from Guizhou and 1 batch in Xinjiang. A total of 81 volatile compounds were screened out in Cordyceps， which could be divided into 13 types （esters， ketones， aldehydes and others） according to the compound structure， indicating that the fishy odor of Cordyceps was a complex odor. There was no significant difference in the types of volatile compounds of Cordyceps from different regions， which suggested that these volatile compounds in Cordyceps produced in Tibet （Naqu）， Qinghai （Yushu and Guoluo） and Sichuan （Litang， Rangtang and Seda） were relatively consistent. However， the contents of some volatile compounds in Cordyceps produced in different regions were quite different， and 16 volatile compounds with significant difference were screened out， including 1-methoxy-2-propyl acetate， <italic>γ</italic>-octalactone， hexyl acetate and others， those compounds maybe could been used as the quality markers for identification of regions of Cordyceps. There was a large difference in volatile compounds between Cordyceps and its counterfeits， and 34 volatile compounds were screened out， including ethyl acetate， acetophenone， 2-ethyl-1-hexanol and others， those compounds maybe could been used as the quality markers for authenticity identification of Cordyceps. Conclusion:In summary， the established method for identifying the fishy odor of Cordyceps in this paper has the characteristics of high sensitivity， accuracy and simplicity， which can provide reference for the analysis of volatile compounds in other Chinese herbal medicines.

Fungicidal activity of volatile organic compounds from Paenibacillus bacteria against Colletotrichum gloeosporioides / Actividad fungicida de compuestos orgánicos volátiles de la bacteria Paenibacillus contra Colletotri chum gloeosporio ides / Atividade fungicida de compostos orgânicos voláteis da bactéria Paenibacillus contra Colletotrichum gloeosporioides

Abstract Some bacteria release volatile organic compounds (VOCs) that can influence the growth of other microorganisms including some pathogens. Identifying bacteria with antifungal activity makes it possible to use such bacteria in the development of biocontrol agents. Thus, the present study focuses on screening VOCs released by eight isolates from Paenibacillus genus, collected at Old Providence and Santa Catalina coral reef (Colombian Caribbean Sea), with antifungal activity against phytopathogenic fungi Colletotrichum gloeosporioides 26B. The VOCs from Paenibacillus sp (PNM-50) showed inhibition rates higher than 50% in the mycelial fungi growth accompanied by macroscopic morphological changes and a reduction in conidiation. In order to identify the VOCs responsible for this antifungal bioactivity, Headspace-Solid Phase Microextraction (HS-SPME) from the bacterial culture was conducted, followed by Gas Chromatography Mass Spectrometry (GC-MS). The chromatographic results revealed a high abundance of VOCs released just by culture media. Once, the difference between VOCs emitted by culture media and bacteria was established, it was possible to make a putative identification of 2-furanmethanol, phenylacetonitrile, and 2,4-dimethylpentanol as possible VOCs responsible for the antifungal activity.

Resumen Algunas bacterias liberan compuestos orgánicos volátiles (COVs) que pueden influir en el crecimiento de otros microorganismos incluyendo algunos patógenos. La identificación de bacterias con actividad antifúngica hace posible el uso de tales bacterias en el desarrollo de agentes de biocontrol. Así pues, en este estudio, se realizó un examen dirigido exclusivamente a los COVs emitidos por ocho aislamientos bacterianos del género Paenibacillus, recolectados en el arrecife de coral de Providencia y Santa Catalina (Mar Caribe colombiano), con actividad antifúngica contra el hongo fitopatógeno Colletotrichum gloeosporioides 26B. Los COVs del aislamiento Paenibacillus sp (PNM-50) mostraron tasas de inhibición superiores al 50% en el crecimiento micelial del hongo, acompañado de cambios morfológicos macroscópicos y una reducción en la conidiación. Para identificar los COVs responsables de esta bioactividad antifúngica, se realizó microextracción en fase sólida del espacio de cabeza (HS-SPME) del cultivo de las bacterias y posterior análisis por cromatografía de gases acoplada a espectrometría de masas (GC-MS). Los resultados cromatográficos revelaron gran abundancia de COVs emitidos por los medios de cultivo. Una vez que se estableció la diferencia entre los COVs emitidos por el medio de cultivo y las bacterias, fue posible identificar tentativamente 2-furanmetanol, fenilacetonitrilo y 2,4-dimetilpentanol como COVs posiblemente responsables de la actividad antifúngica.

Resumo Algumas bactérias liberam compostos orgânicos voláteis (COV) que podem influenciar o crescimento de outros microorganismos, incluindo alguns patógenos. A identificação de bactérias com atividade antifúngica, possibilita seu uso no desenvolvimento de agentes de biocontrole. Neste estudo, foi realizada uma triagem focada nos COV liberados por oito isolados bacterianos do gênero Paenibacillus, coletados nos recifes de coral Old Providence e Santa Catalina (mar do Caribe colombiano), com atividade antifúngica contra fungos fitopatogênicos Colletotrichum gloeosporioides 26B. Os COV de Paenibacillus sp (PNM-50) apresentaram taxas de inibição superiores à 50% sobre o crescimento de fungos miceliais, acompanhadas de alterações morfológicas macroscópicas e redução da conidiação. Para identificar os COV responsáveis por essa bioatividade antifúngica, foi conduzida uma Microextração de Fase Sólida Headspace (HS-SPME) da cultura bacteriana e, em seguida, foi analisada por Cromatografia Gasosa associada à Espectrometria de Massa (GCMS). Os resultados cromatográficos revelaram uma alta abundância de COVs liberados apenas pelos meios de cultura. Uma vez estabelecida a diferença entre os COV emitidos pelos meios de cultura e bactérias, foi possível fazer uma identificação parcial de 2-furanmetanol, fenilacetonitrila e 2,4-dimetilpentanol como possíveis COV responsáveis pela atividade antifúngica.

Antagonistic activity of volatile metabolites from Trichoderma asperellum / 生物工程学报

Trichoderma spp. is a kind of filamentous fungi with important biocontrol value. Twelve strains of Trichoderma spp. were isolated from the soils of different types of crops in Shaoxing, Zhejiang and Foshan, Guangdong. The antagonistic resistance to Fusarium oxysporum was compared by plate confrontation test. The further analysis of volatile secondary metabolites for two strains were carried out using HS-SPME-GC-MS analysis. The results showed that T. asperellum ZJSX5003 and GDFS1009 had fast growth ability, and the inhibition effects on F. oxysporum were 73% and 74% respectively. Six identical volatile metabolites were detected as follows 2-Methyl-1-propanol, 3-Methyl-1-butanol, 3-Methyl-3-buten-1-ol, Acetyl methyl carbinol, Butane-2,3-diol and 6-n-pentyl-2H-pyran-2-one (6-PAP). Among them, 6-PAP was validated to have a higher inhibitory effect on F. oxysporum in vitro. This study will provide basis for the development of biocontrol agents with metabolites of Trichoderma, such as 6-PAP.

Optimization of processing methods for deodorizing Periplaneta americana based on subjective and objective smell evaluation combined with analysis of volatile components / 中草药

Objective: To screen a processing method suitable for deodorizing of Periplaneta americana (PA) through subjective and objective evaluation combined with changes in volatile components, and explore the mechanism of deodorization. Methods: Raw, vinegar-processed, wine-processed, wheat bran-processed products of PA were prepared respectively. Volunteer sensory evaluation combined with electronic nose system was used to evaluate the odor difference between raw and processed products to screen a better processed product. HS-SPME-GC-MS and ROAV were used to analyze the key odorous components of PA. The peak area normalization method combined with multivariate statistical analysis were used to analyze the difference of volatile components between raw and processed products to explore the mechanism of processing. Results|| Volunteer scores showed that the average scores of raw, vinegar-processed, wine-processed, wheat bran-processed products were 3.38, 1.25, 2.88, and 3.04, respectively. The results of the electronic nose showed that the Euclidean distance between the raw and vinegar-processed, wine-processed, wheat bran-processed products were 7.34, 3.77 and 1.60, respectively, but the direction of scatter of vinegar-processed product was opposite to that of wine-processed product and wheat bran-processed product, suggesting that the mechanism of deodorization may be different. Vinegar processing was determined as the optimum method for deodorizing by comprehensive analysis of subjective and objective evaluation data. The key odor components of PA were 3-methyl butanal, hexanal, nonyl aldehyde, heptaldehyde, decyl aldehyde, phenyl acetaldehyde, (E,E)-2,4-nonadienal, 2-pentylfuran, (+)-limonene, and myristic aldehyde. The PCA result of volatile components showed that four kinds of processed products can be clearly distinguished, and there were differences in volatile components and content. There were seven differential chemical components between raw and vinegar-processed products, including hexanal, palmitic acid, oleic acid, acetic acid, ethyl oleate, ethyl palmitate, and ethyl linoleate. The content of vinegar-processed products was lower than that of raw products, especially the key odorous component hexanal. Conclusion: The vinegar processing is a better method to improve the odor of PA, and its mechanism may be associated with reducing odorous components such as hexanal.

Analysis of volatile components of the different Jiuwei Qianghuo preparations by HS-SPME-GC-MS and principal component analysis / 国际药学研究杂志

Objective: To analyze and compare the volatile components of Jiuwei Qianghuo pills, granules and oral liquid. Methods: The volatile components of Jiuwei Qianghuo pills, granules and oral liquid were analyzed and compared by the head-space solid-phase microextraction and gas chromatography-mass spectrometry(HS-SPME-GC-MS), the relative percentage of each component was calculated using the area normalization method, and the principal component analysis was also performed. Results: A total of 90 kinds of volatile components were identified from Jiuwei Qianghuo pills, accounting for 97.19% of the total volatile components; 27 kinds of volatile components were identified from Jiuwei Qianghuo granules, accounting for 92.92% of the total volatile components;22 kinds of volatile components were identified from Jiuwei Qianghuo oral liquid, accounting for 87.60% of the total volatile components. A total of 111 volatile components were identified in the three preparations, of which 6 were common components, but the contents of the common components were different. The specific components of the pills, granules and oral liquid were 68, 8 and 13, respectively. Moreover, the comprehensive scores of the three dosage forms in the principal component analysis showed a large difference, with the high, middle and low values for the pills, granules and oral liquid, respectively. Conclusion: The composition and content of volatile components were different in the Jiuwei Qianghuo pill, granule and oral liquid preparations. From the point of view of the volatility, the comprehensive score of Jiuwei Qianghuo pills is higher than that of granules and oral liquid.

Multivariate optimization of a HS-SPME/GC-MS technique for the characterization of volatile compounds present in Hedeoma multiflorum Benth / Optimización Multivariada de una técnica HS-SPME/GC para la caracterización de los compuestos volátiles presentes en Hedeoma multiflorum Benth

The aim of the present work was to optimize the main experimental variables of a procedure using HS-SPME/GC-MS as the analytical methodology to establish the profile of the volatile compounds present in aerial parts of Hedeoma multiflorum Benth. The influence of the type of fiber, equilibrium time, extraction time and extraction temperature on the composition of the volatile compounds was determined using response surface methodology (RSM), and the parameters of the models were corroborated by multiple linear regressions. The results showed that the regression models generated adequately explained the data variation and represented the relationships between the parameters and their responses. The optimal analysis conditions from the contour plots were established (DVB/CAR/PDMS fiber, with a 10 min equilibrium time, 10 min extraction time, and 40°C). Under these conditions, 41 volatile components in the whole plant were determined, which represents more than those reported using hydrodistillation.

El objetivo del presente trabajo fue optimizar las principales variables experimentales de un procedimiento HS-SPME/GC para establecer el perfil de compuestos volátiles presentes en la parte aérea de Hedeoma multiflorum Benth. Se determinó la influencia de las variables tipo de fibra, tiempo de equilibrio, tiempo de extracción y temperatura de extracción sobre la composición de los volátiles, utilizando una met odología de superficie de respuesta (RSM) y los parámetros del modelo se corroboraron por regresión lineal múltiple. Los resultados demostraron que los modelos de regresión generados explican adecuadamente la variación de los datos y representaron significativamente las relaciones reales entre los parámetros y sus respuestas. Las condiciones óptimas de análisis fueron establecidas (DVB/CAR/PDMS, con un tiempo de equilibrio de 10 minutos, un tiempo de extracción de 10 minutos y trabajando a 40°C). Utilizando esta metodología, se determinaron 41 componentes volátiles en planta entera, más que los reportados mediante hidrodestilación.

Percepção sensorial do off-odor em carnes bovinas irradiadas em embalagens á vácuo contendo carvão ativado / Off-odor perception in irradiated beef vacuum packaged with charcoal

Objetivou-se avaliar a utilização de carvão ativo na redução de compostos voláteis responsáveis pelo off-odor de carnes bovinas irradiadas. Para tal, contrafilés bovinos, embalados a vácuo, com e sem carvão ativo, e irradiados (1, 2 e 3 kGy), foram analisados quanto a formação de compostos de enxofre e quanto a percepção sensorial de off-odor. O único composto de enxofre identificado nas amostras foi o dimetil sulfeto (DMS), sendo encontrado em menor concentração nas amostras irradiadas com carvão ativo na embalagem. Independentemente da utilização do carvão, os painelistas perceberam o off-odor das carnes irradiadas em qualquer dose quando comparado à carne não-irradiada. Quando foi comparado as carnes irradiadas com carvão em relação àquelas irradiadas sem carvão, os painelistas foram capazes de identificar o off-odor apenas nas amostras irradiadas com 1 kGy. Conclui-se que o carvão ativo reduziu a concentração de DMS na embalagem de carnes irradiadas.

Volatile compounds and quality analysis in commercial medicinal plants of Camellia sinensis / Caracterização dos compostos voláteis e análise da qualidade de plantas medicinais comerciais de Camellia sinensis

ABSTRACT: The interest in the use of green tea (Camellia sinensis) (L.) Kuntze (Theaceae) products have increased in the last few years due to its medicinal properties. In the present study, we proposed that headspace solid phase microextraction, in combination with gas chromatography coupled to mass spectrometric could be an efficient method to assess the volatile compounds and to ensure the quality control of C. sinensis. We have also compared the anatomical leaf of different commercial green tea samples, analyzed the information in their labels and determined the presence of foreign materials, moisture content, total ashes and microorganisms. Among the 30 analyzed samples, six were identified as C. sinensis according to the anatomical study; 83.4% were not in accordance with the specified limits for foreign matter and 6.6% for moisture content. All samples presented total ashes in accordance with the current legislation. The analysis indicated the presence of several different volatile organic compounds, being terpenes, hydrocarbons and alcohols the major ones. Microbiological analysis showed that 13.3% and 16.6% of the samples exceeded the limits for counts of molds and yeasts, and for mesophilic bacteria, respectively. 73.3% presented E. coli above the established sanitary limits.

RESUMO: O interesse no chá verde comercial (Camellia sinensis) (L.) Kuntze (Theaceae) tem aumentado nos últimos anos devido suas propriedades medicinais. No presente estudo utilizamos a microextração em fase sólida, em combinação com a cromatografia gasosa acoplada com espectrometria de massas, como um eficiente método de caracterização de compostos voláteis e efetuamos o controle de qualidade de C. sinensis. Comparamos também a anatomia das folhas de diferentes amostras comerciais de chá verde, as informações de seus rótulos e determinamos a presença de matérias estranhas, de microrganismos, o teor de umidade e de cinzas totais. Entre as trinta amostras analisadas, seis foram identificadas como C. sinensis de acordo com o estudo anatômico; 83,4% não estavam de acordo com os limites especificados para matérias estranhas e 6,6% para o teor de umidade. Todas as amostras apresentaram cinzas totais de acordo com a legislação vigente. As análises evidenciaram diversos compostos orgânicos voláteis distintos, sendo majoritários terpenos, hidrocarbonetos e álcoois. As análises microbiológicas mostraram que 13,3 e 16,6% das amostras excedeu os limites de contagem para bolores e leveduras, e para bactérias mesófilas, respectivamente. Por fim, 73,3% das amostras apresentou Escherichia coli acima dos limites sanitários estabelecidos.

Analysis of anti-inflammation mechanism of zukamu granules based on network pharmacology and hs-spme-gc-ms / 国际药学研究杂志

Objective: To explore the material basis and anti-inflammatory mechanisms of Zukamu granules (ZKMG)based on the headspace-solid phase microextraction-gas chromatography-mass spectrometry(HS-SPME-GCMS) technique and network pharmacology analyses. Methods: HS-SPME-GC-MS technique was used to extract and identify the volatile components of ZKMG. Then combined with the non-volatile components obtained by literature retrieval, we constructed the main chemical composition table. The bioactive components were screened based on the Traditional Chinese Medicine Systems Pharmacology Database and Analysis Platform(TCMSP), and their targets were predicted by the Swiss Target Prediction database. Thereafter, the anti-inflammatory-related targets were screened based on the Thera- peutic Targets Datebase and DrugBank with”Anti-inflammatory”as keyword. Then, the STRING database to analyze protein-protein interaction(PPI)and the software of Cytoscape 3.6.1 was used to construct the component-target-antiinflammatory target network. Finally, enrichment of function and signaling pathways of the target genes was conducted by Gene Ontology(GO)database and the Database for Annotation, Visualization and Integrated Discovery(DAVID). Re- sults: Thirty bioactive components including thymol, kaempferol and quercetin in ZKMG were screened out. Ninety-seven targets were predicted and AKR1B1, ALOX15, ALOX5, CYP1A2, EGFR, CHRM1, NOS3, PLA2G1B, PTGS2, BCHE were key anti-inflammatory targets. Sixty-eight pathways related to anti-inflammation were obtained by KEGG enrichment analysis, mainly including arachidonic acid metabolism, MAPK signaling pathway, inflammatory mediator regulation of TRP channels, IL-17 signaling pathway and NF-κB signaling pathway. Conclusion: This study focuses on the chemical constituents of ZKMG and network pharmacology to predict the material basis and pharmacological mecha- nism of their anti-inflammatory effect, which lays a good foundation for the verification of the later biological experiments and provides certain reference basis for the research on the anti-inflammation mechanism of other compound preparations.

Analysis and identification of volatile constituents in different parts of Murrayae Folium et Cacumen by HS-SPME-GC-MS / 国际药学研究杂志

Objective: To analyze,identify and compare the volatile components in different medicinal parts of Murrayae Folium et Cacumen(Kamuning). Methods: The volatile components were extracted by headspace solid-phase microextraction(HS-SPME)and analyzed by gas chromatography-mass spectrometry(GC-MS). The relative contents were calculated for each of the volatile components by the area normalization method. Results A total of 74 compounds were identified in the root,stem and leaf of Murrayae Folium et Cacumen,among which there were 8 components in common in the three parts,and the numbers of specific components in roots,stems and leaves were 23,27 and 32,respectively. Conclu- sion The present HS-SPME-GC-MS method was suitable for the analysis of volatile components in the different parts of Murrayae Folium et Cacumen. Some volatile components were identified to be medicinal ingredients. The present results provide a reference for further development and application of the Murrayae Folium et Cacumen resources.

Detection of ketamine, MDMA and their main metabolites in urine samples by SPME-HPLC-MS / 中国药科大学学报

@#To establish a method for the determination of ketamine and MDA and their main metabolites in urine by solid phase microextraction-liquid chromatography-mass spectrometry. In a urine sample supplemented with quantitative ketamine, norketamine, MDMA and MDA control. The solution was adjusted pH 11, added solid Na2CO3, heated and stirred at 60 °C. Then, the sample was extracted by SPME with 60 μm polydimethylsiloxane-vinylbenzene copolymer(PDMS/DVB ), a middle-polar coated fiber for 15 minutes and then analyzed by HPLC-MS. The result showed good linearity in the range of 0. 03-1. 0 μg/mL, r≥0. 999 2, and LOD was 0. 01 μg/mL, the value of the average recovery rate was varying from 97. 19%-105. 44%, and RSD was within 10%. The method is simple, safe and accurate, and can be used to determine ketamine, MDMA and their main metabolites in urine.

Characteristics Analysis for Volatile Compounds of 18 Heat-Clearing Herbs / 中国实验方剂学杂志

Objective: Headspace-solid phase microextraction-gas chromatography-mass spectrometry (HS-SPME-GC-MS) was used to analyze the characteristic volatile compounds from 18 heat-clearing herbs. Method: HS-SPME was used to extract the volatile components from different heat-clearing herbs,and the chemical compositions were analyzed by GC-MS. The GC was performed at the injector temperature of 250℃,the high-purity helium was used as the carrier gas at a constant column flow of 1.0 mL·min-1 with no split sampling. The solvent delay time was 3 min. Mass spectrum conditions included electron bombardment ion source,electron bombardment energy of 70 eV,ion source temperature of 230℃,quadrupoles temperature of 150℃,and scanning range of m/z 29-370.The volatile components were confirmed according to NIST2013 database,and the relative content percentage of each component was calculated by peak area normalization method. PCA was used to detect clustering and discuss the characteristics of volatile compounds of 18 heat-clearing herbs. Result: A total of 328 volatile compounds were detected in 18 heat-clearing herbs,including alkanes,unsaturated hydrocarbon,alcohols,aldehyde,ketones,esters,furan and other unknown compounds. The number and relative content of volatile components in different heat-clearing herbs varied dramatically. Several important characteristic volatile compounds,such as l-camphor,torreyol,caryophyllene oxide,globulol and 2,4-cycloheptadien-1-one,2,6,6-trimethyl,were detected in the 18 heat-clearing herbs by principal component analysis. Conclusion: Heat-clearing herbs contains rich volatile components,which are the main contributors to the formation of unique aroma of herbs,as well as the main active substances.

Analysis of Volatile Components of Different Processed Products of Curcuma wenyujin Radix by HS-SPME-GC-MS / 中国实验方剂学杂志

Objective:To analyze and compare volatile components in raw and fried products of Curcuma wenyujin radix, and find out the material basis for the differences in efficacy between them,in order to provide powerful support and reference for the rational use of C. wenyujin radix of different processed products and establish a more perfect quality evaluation system. Method:HS-SPME combined with GC-MS was used to analyze and compare volatile components and relative percentage in different processed products of C. wenyujin radix. Result:Totally 42 peaks were detected from the raw product of C. wenyujin radix,and 23 components were identified. Totally 59 peaks were detected from vinegar-baked C. wenyujin radix,and 34 components were identified. Totally 64 peaks were detected from wine-baked C. wenyujin radix,and 40 components were identified. Compared with C. wenyujin radix,22 kinds of new ingredients were produced. Compared with C. wenyujin radix,29 kinds of new ingredients were produced in wine-baked C. wenyujin radix. The composition and content of volatile components in different processed products of C. wenyujin radix were changed. Conclusion:The headspace solid phase micro-extraction method is simple in operation and fast in extraction speed,with no use of organic solvent, no pollutant in the environment and a low operation cost. The method using headspace solid phase micro-extraction combined with gas chromatography-mass spectrometry has a high stability and reliability. It is suitable for rapid analysis of volatile components between C. wenyujin radix and its different processed products. It can provide a scientific basis for the quality evaluation of C. wenyujin radix and its different processed products,and a scientific reference for the rational use of C. wenyujin radix resources.

Analysis and identification of volatile components of different parts of Clausena lansium in Hainan by HS-SPME-GC-MS / 中草药

Objective A headspace-solid phase microextraction-gas chromatography-mass spectrometry method (HS-SPME-GC-MS) was adopted for analyzing the volatile components of different parts of Clausena lansium in Hainan Province. Methods Five different fibers were investigated and optimized. Other five experimental parameters such as volume of water, extraction temperature, equilibrium time, extraction time, and salt concentration had been evaluated and optimized by means of the orthogonal design with L16(45) table. Finally, the volatile components of C. lansium leaves, pericarps, and seeds in Hainan were analyzed and identified by GC-MS combined with retention index (RI). Results The optimum extraction conditions were as follows: a 50/30 μm DVB/CAR/PDMS fiber, 10 mg sample powders, 2.0 mL water, 0.2 g NaCl, extraction temperature 80 ℃, equilibrium time 30 min, extraction time 60 min. A total of 83 chemical components were identified from leaves, 96 from pericarps, and 106 from seeds, representing the relative contents of 95.24%, 92.15%, and 95.92% of the total composition. The highest contents were sesquiterpenes in all of the parts, but there were obviously different both in components and contents. Conclusion The HS-SPME-GC-MS method is rapid and sensitive, with a small sample size, without any organic solvents. GC-MS combined with RI has improved the accuracy of analysis and identification. The results may provide experimental basis for further exploitation of C. lansium in Hainan. This method can be used to perform enrichment analysis of the components with high-boiling point and micro-components, which can comprehensively and scientifically characterize and evaluate the quality of Chinese materia medica.

Analysis of Volatile Components in Smilax Glabra Robx. and Its Adulterant / 中国药师

Objective: To analyze and compare the volatile components in Smilax glabra Robx. and its adulterant Smilax china L. . Methods: The volatile components in Smilax glabra Robx. and Smilax china L. were analyzed by head space solid phase micro-extraction (HS-SPME) combined with gas chromatography-mass spectrometry ( GC-MS). The relative percentage of each component was calculated by area normalization method. Results: Totally 24 components were detected out from Smilax glabra Robx. , and among them, 20 components were identified, which accounted for 97. 04% of the volatile components. Totally 21 components were detected out from Smilax china L. , and among them, 15 components were identified, which accounted for 77. 76% of the volatile components. Conclusion: The composition and content of volatile components in Smilax glabra Robx. and its adulterant Smilax china L. are differ-ent. The method can provide scientific basis for the identification of Smilax glabra Robx. and its adulterants.

Analysis of Volatile Compounds Extracted from Dipsaci Radix and Its Wine Broiled Products by GC-MS / 中国药师

Objective: To analyze the composition and the content of volatile components in Dipsaci Radix and its wine broiled products. Methods: Headspace solid phase microextraction (HS-SPME) combined with gas chromatography-mass spectrometry ( GC-MS) was used to analyze the volatile components in Dipsaci Radix and its wine broiled products. The area normalization method was used to calculate the relative content. Results: Totally 31 ingredients were identified, which mainly included phenols, olefins, alcohols and aldehydes. Totally 25 peaks were detected out from the volatile components in Dipsaci Radix, and among them, 22 components were identified, which accounted for 94. 74% of the total volatile components. The content of 5-allylguaiacol was the highest, which accounted for 28. 37% of the total volatile components. Totally 23 peaks were detected out from the volatile components in wine-pro-cessed Dipsaci Radix, and among them, 17 ingredients were identified, which accounted for 85. 92% of the total volatile components. The content of nonanal was the highest, which accounted for 9. 66% of the total volatile components. Conclusion: The composition and the content of volatile components in Dipsaci Radix and its wine broiled products are different. The experiment provides scientific reference for the further research and development of the volatile components in Dipsaci Radix and its wine broiled products.