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1.
Journal of Forensic Medicine ; (6): 144-150, 2023.
Article in English | WPRIM | ID: wpr-981848

ABSTRACT

OBJECTIVES@#To identify 1-(4-fluorophenyl)-2-(1-pyrrolidinyl) pentan-1-one (4-F-α-PVP) analog 1-(4-fluoro-3-methyl phenyl)-2-(1-pyrrolidinyl) pentan-1-one (4-F-3-Methyl-α-PVP) hydrochloride without reference substance.@*METHODS@#The direct-injection electron ionization-mass spectrometry (EI-MS), GC-MS, electrospray ionization-high resolution mass spectrometry (ESI-HRMS), ultra-high performance liquid chromatography-high resolution tandem mass spectrometry (UPLC-HRMS/MS), nuclear magnetic resonance (NMR), ion chromatography and Fourier transform infrared spectroscopy (FTIR) were integrated utilized to achieve the structural analysis and characterization of the unknown compound in the sample, and the cleavage mechanism of the fragment ions was deduced by EI-MS and UPLC-HRMS/MS.@*RESULTS@#By analyzing the direct-injection EI-MS, GC-MS, ESI-HRMS and UPLC-HRMS/MS of the compound in the samples, it was concluded that the unknown compound was a structural analog of 4-F-α-PVP, possibly with one more methyl group in the benzene ring. According to the analysis results of 1H-NMR and 13C-NMR, it was further proved that the methyl group is located at the 3-position of the benzene ring. Since the actual number of hydrogen in 1H-NMR analysis was one more than 4-F-3-Methyl-α-PVP neutral molecule, it was inferred that the compound existed in the form of salt. Ion chromatography analysis results showed that the compound contained chlorine anion (content 11.14%-11.16%), with the structural analysis of main functional group information by FTIR, the unknown compound was finally determined to be 4-F-3-Methyl-α-PVP hydrochloride.@*CONCLUSIONS@#A comprehensive method using EI-MS, GC-MS, ESI-HRMS, UPLC-HRMS/MS, NMR, ion chromatography and FTIR to identify 4-F-3-Methyl-α-PVP hydrochloride in samples is established, which will be helpful for the forensic science laboratory to identify this compound or other analog compounds.


Subject(s)
Benzene , Gas Chromatography-Mass Spectrometry/methods , Spectrometry, Mass, Electrospray Ionization , Chromatography, High Pressure Liquid/methods
2.
Braz. J. Pharm. Sci. (Online) ; 59: e23011, 2023. tab, graf
Article in English | LILACS | ID: biblio-1505852

ABSTRACT

Abstract Oil-in-water photoprotective nanoemulsions (NEs) were developed using Babassu (BBS) lipophilic extract, nonionic surfactants, and low concentrations of organic sunscreens by ultrasonic processing. BBS extract was chosen due to its suitable physicochemical properties (acidity index, peroxide index, refraction index, and relative density) and predominance of saturated fatty acids, identified by gas chromatography-mass spectrometry (GC-MS), which promote biological activities and high oxidative stability. NEs were characterized by mean droplet size, morphology, polydispersity index (PdI), pH, and organoleptic properties, and the physical stability of the NEs was evaluated for 120 days at room temperature. The sun protection factor (SPF) was determined, and the photostability and in vitro cytotoxicity assays were performed for NEs. All NEs remained stable for 120 days, with a droplet size <150 nm and a monomodal distribution profile. The pH values were compatible with the skin's pH. NE3 showed a spherical morphology, with a mean droplet size of 125.15 ± 0.16 nm and PdI of 0.145 ± 0.032. NE3 containing BBS extract and sunscreens presented an SPF of 35.5 ± 3.0, was photostable after 6 h of radiation and was non-cytotoxic to fibroblast cells. Thus, NE3 could be considered a promising formulation for developing synergic plant-extract sunscreen photoprotective products for the market


Subject(s)
Plants/adverse effects , Sunscreening Agents/pharmacology , Plant Extracts/agonists , Arecaceae/classification , Vegetable Fats , In Vitro Techniques/methods , Sun Protection Factor/classification , Gas Chromatography-Mass Spectrometry/methods
3.
Journal of Forensic Medicine ; (6): 457-464, 2023.
Article in English | WPRIM | ID: wpr-1009378

ABSTRACT

OBJECTIVES@#To establish the GC-MS qualitative and quantitative analysis methods for the synthetic cannabinoids, its main matrix and additives in suspicious electronic cigarette (e-cigarette) oil samples.@*METHODS@#The e-cigarette oil samples were analyzed by GC-MS after diluted with methanol. Synthetic cannabinoids, its main matrix and additives in e-cigarette oil samples were qualitatively analyzed by the characteristic fragment ions and retention time. The synthetic cannabinoids were quantitatively analyzed by using the selective ion monitoring mode.@*RESULTS@#The linear range of each compound in GC-MS quantitative method was 0.025-1 mg/mL, the matrix recovery rate was 94%-103%, the intra-day precision relative standard deviations (RSD) was less than 2.5%, and inter-day precision RSD was less than 4.0%. Five indoles or indazole amide synthetic cannabinoids were detected in 25 e-cigarette samples. The main matrixes of e-cigarette samples were propylene glycol and glycerol. Additives such as N,2,3-trimethyl-2-isopropyl butanamide (WS-23), glycerol triacetate and nicotine were detected in some samples. The content range of synthetic cannabinoids in 25 e-cigarette samples was 0.05%-2.74%.@*CONCLUSIONS@#The GC-MS method for synthesizing cannabinoid, matrix and additive in e-cigarette oil samples has good selectivity, high resolution, low detection limit, and can be used for simultaneous qualitative and quantitative analysis of multiple components; The explored fragment ion fragmentation mechanism of the electron bombardment ion source of indole or indoxamide compounds helps to identify such substances or other compounds with similar structures in cases.


Subject(s)
Gas Chromatography-Mass Spectrometry/methods , Electronic Nicotine Delivery Systems , Illicit Drugs/analysis , Indazoles/chemistry , Glycerol/analysis , Cannabinoids , Indoles/chemistry , Ions
4.
China Journal of Chinese Materia Medica ; (24): 676-683, 2022.
Article in Chinese | WPRIM | ID: wpr-927950

ABSTRACT

The volatile oil of Chuanxiong Rhizoma(CX) is known as an effective fraction. In order to seek a suitable method for processing CX and its decoction pieces, this study selected 16 volatile components as indices to investigate how different processing methods such as washing/without washing, sun-drying, baking, oven-drying and far-infrared drying at different temperatures affected the quality of CX and its decoction pieces(fresh CX was partially dried, cut into pieces, and then dried) by headspace gas chromatography-mass spectrometry(GC-MS), cluster analysis, principal component analysis and comprehensive weighted scoring. The results showed that the rapid washing before processing did not deteriorate the volatile components of CX. Considering the practical condition of production area, oven-drying was believed to be more suitable than sun-drying, baking, and far-infrared drying. The CX decoction pieces with a thickness of 0.3-0.4 cm were recommended to be oven-dried at 50 ℃. The integrated processing(partial drying, cutting into pieces, and drying) did not cause a significant loss of volatile components. For the fresh CX, the oven-drying at 60 ℃ is preferred. The temperature should not exceed 60 ℃, and drying below 60 ℃ will prolong the processing time, which will produce an unfavorable effect on volatile components. This study has provided the scientific evidence for field processing of CX, which is conducive to realizing the normalization and standardization of CX processing in the production area and stabilizing the quality of CX and its decoction pieces.


Subject(s)
Desiccation , Gas Chromatography-Mass Spectrometry/methods , Oils, Volatile , Principal Component Analysis , Rhizome/chemistry , Volatile Organic Compounds/analysis
5.
Braz. J. Pharm. Sci. (Online) ; 58: e20253, 2022. tab, graf
Article in English | LILACS | ID: biblio-1403711

ABSTRACT

Abstract Formaldehyde is a carcinogenic compound used as preservative in cosmetic products. In this study, a derivatization procedure using MeOH, EtOH and HCl (25:25:1), and incubation at 60ºC for 4 hours was optimized, and the derivatized products - methylal, ethoxymethoxymethane (EMM), and ethylal - were directly analyzed by headspace-gas chromatography-mass spectrometry (HS-GC-MS) to determine formaldehyde concentrations. The validated method provided good linearity of the standard curve, selectivity, recovery (89.6-106.6%), repeatability, and intermediate precision (RSD < 12%), with an LOD of 0.0015% and an LOQ of 0.005% for all derivatized analytes. The validated method showed to be fast, clean, and easy to implement in a laboratory. To the best of our knowledge, this is the first reported HS-GC-MS procedure to determine formaldehyde as methylal, ethylal, and EMM as derivatized compounds. The method was satisfactorily applied for the analysis of nine hair-straightener cream samples seized by the Civil Police of the Federal District, Brazil. Eight samples contained formaldehyde, at levels ranging from 0.33 to 4.02 %, higher than the legal levels, indicating the need to control the levels of this toxic compound in cosmetic products


Subject(s)
Cosmetics/analysis , Formaldehyde/analysis , Gas Chromatography-Mass Spectrometry/methods , Civil Police/legislation & jurisprudence , Acetals/agonists , Methods
6.
Braz. J. Pharm. Sci. (Online) ; 58: e20417, 2022. tab, graf
Article in English | LILACS | ID: biblio-1403712

ABSTRACT

Abstract Schinus terebinthifolia Raddi green fruits essential oil (EO) was evaluated regarding its phytochemical profile, antimicrobial and cytotoxic activities, and toxicity. Gas chromatography with mass spectrometry was applied to identify its constituents, thereafter the minimum inhibitory concentration, minimum bactericidal and fungicidal concentrations, and its antibiofilm activity were evaluated. The EO cytotoxicity was assessed in tumor and non-tumor human cells, and in vivo toxicity was evaluated in a Galleria mellonella model. The major constituents of S. terebinthifolia EO were alpha-phellandrene and beta-phellandrene. The EO had a weak activity against all strains of Candida albicans (MIC 1000µg/mL) and had no activity against non-albicans strains, bacteria, and C. albicans biofilm. Cytostatic activity against all tumor cell lines was shown. Additionally, cell viability remained at EO concentrations up to 62.5 µg/mL. At 16 mg/mL, 50% hemolysis was observed, and it had low toxicity in vivo. Overall, the S. terebinthifolia EO was characterized by low antimicrobial and antibiofilm activities, with no evidence of toxicity to human tumor and non-tumor cells


Subject(s)
Oils, Volatile/analysis , Anacardiaceae/anatomy & histology , Fruit/classification , Plants, Medicinal/adverse effects , Toxicity , Gas Chromatography-Mass Spectrometry/methods
7.
Braz. J. Pharm. Sci. (Online) ; 58: e20464, 2022. tab, graf
Article in English | LILACS | ID: biblio-1403751

ABSTRACT

Abstract Papaveraceae is one of the prominent alkaloid-containing families, and plants of the genus Glaucium (Papaveraceae) are known for their bioactive alkaloids. Glaucium species have been used in traditional medicine in Turkey as an analgesic, narcotic, sedative, and antitussive. In this study, it was planned to evaluate the inhibitory activity of an alkaloidal extract of Glaucium corniculatum subsp. refractum on acetylcholinesterase (AChE), butyrylcholinesterase (BuChE) and prolyl oligopeptidase (POP), as well as exploring the chemical profile of the plant by using Gas Chromatography-Mass Spectrometry (GC-MS). The AChE, BuChE and POP inhibition activities of the alkaloidal extract of G. corniculatum subsp. refractum were determined spectrophotometrically. A rapid GC-MS method was used to identify alkaloids that could be responsible for these inhibition activities. In total, eleven alkaloids were identified in the alkaloid extract of the plant by GC-MS. Allocyptopine (52.92%) and protopine (25.38%) were found as the major constituents. The alkaloidal extract of G. corniculatum subsp. refractum showed potent AChE inhibitory activity (IC50:1.25 µg/mL) and BuChE inhibitory activity (IC50: 7.02 µg/mL). The extract also showed a remarkable inhibitory effect on POP with an IC50 value of 123.69 µg/mL. This study presents the first GC-MS investigation and POP inhibitory activity of G. corniculatum subsp. refractum.


Subject(s)
Acetylcholinesterase/adverse effects , Butyrylcholinesterase/adverse effects , Papaveraceae/metabolism , Plant Extracts/agonists , Alkaloids/analysis , Gas Chromatography-Mass Spectrometry/methods , Medicine, Traditional
8.
Braz. J. Pharm. Sci. (Online) ; 58: e20735, 2022. tab, graf
Article in English | LILACS | ID: biblio-1420479

ABSTRACT

Abstract Herein the chemical constituents and the anti-pain properties of the essential oil from the stem bark of Casuarina equisetifolia L. (Casuarinaceae) grown in Nigeria were evaluated. The essential oil was obtained by hydrodistillation method in an all glass Clevenger-type apparatus, and characterized by gas chromatography (GC-FID) and gas chromatography-mass spectrometry (GC-MS). The hot plate method was used to determine the anti-nociceptive property whereas the anti-inflammatory activity was evaluated by carrageenan-induced and formalin experimental models. The pale-yellow essential oil was obtained in yield of 0.21% (v/w), calculated on a dry weight basis. The main constituents of the essential oil were methyl salicylate (30.4%), a-zingiberene (15.5%), (E)-anethole (9.5%), b-bisabolene (8.6%), b- sesquiphellandrene (6.9%), and ar-curcumene (6.2%). In the anti-nociceptive study, the rate of inhibition increases as the doses of essential oil increases with optimum activity at the 30th and 60th min for all tested doses. The essential oil displayed anti-nociceptive activity independently of reaction time at the highest tested dose (200 mg/kg). The essential oil of C. equisetifolia moderately reduced pain responses in early and late phases of the formalin test. The oil inhibited the paw licking in the neurogenic phase (60-63%) compared to the late phase of the formalin test. The carrageenan- induced oedema model revealed the suppression of inflammatory mediators within the 1st - 3rd h. Thus, C. equisetifolia essential oil displayed both anti-nociceptive and anti-inflammatory activities independent of the dose tested. The anti-inflammatory and anti-nociceptive activities of C. equisetifolia essential oil are herein reported for the first time


Subject(s)
Animals , Male , Rats , Oils, Volatile/analysis , Plant Stems/anatomy & histology , Plant Bark/classification , Analgesics/pharmacology , Anti-Inflammatory Agents/pharmacology , Carrageenan/adverse effects , Chromatography, Gas/methods , Microscopy, Electron, Scanning Transmission/methods , Gas Chromatography-Mass Spectrometry/methods
9.
Braz. J. Pharm. Sci. (Online) ; 58: e181097, 2022. tab, graf
Article in English | LILACS | ID: biblio-1374562

ABSTRACT

Abstract Essential oils from four Ocotea species collected in southern Brazil were evaluated for chemical composition using gas chromatography coupled with mass spectrometry. The primary compound identified in O. acutifolia essential oil was an unsaturated tetracyclic diterpene, phyllocladene (67.7%), followed by a sesquiterpene hydrocarbon, ß-selinene (18.0%). The sesquiterpene fraction was predominant in oils from two collections of O. puberula; ß-caryophyllene (25.2%) and globulol (22.6%) were the major compounds identified in collections 1 and 2, respectively. O. silvestris essential oil contained predominantly germacrene D and bicyclogermacrene. These compounds were also predominant in essential oil from O. indecora leaves collected from shady habitats. By contrast, essential oil extracted from O. indecora grown under direct sunlight contained mainly oxygenated sesquiterpenes, such as guaiol (30.2%), α-eudesmol (27.6%), and ß-eudesmol (12.7%). Chemotaxis assays showed that Ocotea essential oils had no significant inhibitory activity on leukocyte migration compared with a chemotactic stimulant (lipopolysaccharide from Escherichia coli). However, the oils exhibited antifungal activity against Candida parapsilosis, with a minimum inhibitory concentration of 500 µg/mL. To our knowledge, this is the first study to investigate the in vitro antifungal and antichemotactic activities of essential oils from Ocotea species native to southern Brazil


Subject(s)
Oils, Volatile/chemistry , Ocotea/anatomy & histology , Biological Products , Ecosystem , Lauraceae/classification , Candida parapsilosis , Gas Chromatography-Mass Spectrometry/methods
10.
Braz. J. Pharm. Sci. (Online) ; 58: e19118, 2022. tab
Article in English | LILACS | ID: biblio-1374566

ABSTRACT

Abstract The chemically complex essential oils of Baccharis species are associated with several biological activities, such as antimicrobial and antiulcerous properties. However, few studies have investigated Baccharis erioclada DC. Therefore, in this study, we aimed to characterize the essential oil of B. erioclada and evaluate its antioxidant, antimicrobial, and hemolytic potential. The essential oil was extracted by hydrodistillation using a Clevenger apparatus and analyzed via gas chromatography-mass spectrometry (GC-MS). Phosphomolybdenum complex formation, reducing antioxidant power, and thiobarbituric acid reactive substances (TBARS) methods were used to determine antioxidant potential. To evaluate the essential oil's antimicrobial activity, minimum inhibitory concentrations (MIC) in Staphylococcus aureus, Escherichia coli, Pseudomonas aeruginosa, and Candida albicans were calculated. Hemolytic activity was determined in sheep red blood cells. Thirty-one compounds were identified via GC-MS analysis, representing 81.60% of the total essential oil. These compounds included: turmerone (27.97%), fokienol (13.47%), ledol (9.78%), and santalol (5.35%). The class of compounds identified was the oxygenated sesquiterpenes (62.52%). Antioxidant activity was confirmed via phosphomolybdenum complex formation and TBARS methods. Moderate antimicrobial activity and low hemolysis rates were displayed at concentrations of 250 and 500 µg/mL


Subject(s)
Oils, Volatile/analysis , Baccharis/anatomy & histology , Antioxidants/pharmacology , Microbial Sensitivity Tests/instrumentation , Asteraceae/classification , Gas Chromatography-Mass Spectrometry/methods
11.
Cienc. tecnol. salud ; 9(2): 133-149, 2022. il 27
Article in Spanish | LILACS, DIGIUSAC, LIGCSA | ID: biblio-1413160

ABSTRACT

Se comparan las métricas de 37 modelos climáticos globales (GCMs, por sus siglas en inglés) de la Fase 6 del Proyecto de Intercomparación de Modelos Acoplados (CMIP6) con el objetivo de simular el clima de Guatemala del periodo de 1971 al 2014. La temperatura y precipitación mensual fue comparada con los datos de observación de la Unidad De Investigación Climática de la Universidad del este de Anglia (CRU). Se generó un ranquin de modelos basado en la menor distancia entre tres dimisiones basado en tres métricas; Coeficiente de Correlación de Pearson (CCP), Error medio cuadrático (RMSE) y Desviación estándar (DS). Este ordenamiento coincide con los mejores valores de eficiencia Nash-Sutcliffe (NSE) para temperatura y eficiencia Kling-Gupta (KGE) para la precipitación, demás se calculan las métricas; coeficiente de correlación de Spearman (CCS), errores de sesgo medio (MBE) y el absoluto medio (MAE). Para precipitación los primeros 5 modelos presentan valores KGE de entre 0.5 y 0.7, el CCP y CCS entre 0.7 a 0.8 comparados con CRU. Para temperatura los primeros 5 modelos presenta valores de NSE de entre 0.5 a 0.6, CCP y CCS de 0.8. Los modelos sobreestiman levemente la temperatura y subestiman la precipitación. Los modelos con mejor habilidad fueron CIESM para temperatura¼ y el modelo IPSL-CM6A-LR para precipitación. Adicionalmente se compara el promedio de 66 estaciones locales con CRU, presentando un KGE de 0.51, CCP de 0.77 para precipitación y NSE de -0.17 y un CCP de 0.20 para temperatura. Finalmente, se presenta una tabla con los 10 primeros modelos para cada variable.


Metrics from 37 global climate models (GCMs) from Phase 6 of the Coupled Model Intercomparison Project (CMIP6) with the purpose of simulating the climate of Guatemalan from 1971 to 2014. Monthly temperature and precipitation were compared with data from observation of the Climatic Research Unit of the University of East Anglia (CRU). A ranking of models was generated based on the shortest distance between three resignations based on three metrics; Pearson's Correlation Coefficient (PCC), Root Mean Square Error (RMSE), and Standard Deviation (SD). This ordering coincides with the best values of Nash-Sutcliffe efficiency (NSE) for temperature and Kling-Gupta efficiency (KGE) for precipitation; other metrics are calculated; Spearman's correlation coefficient (CCS), mean bias errors (MBE), and mean absolute error (MAE). For precipitation, the first 5 models present KGE values between 0.5 and 0.7, the CCP and CCS between 0.7 and 0.8 compared to CRU. For temperature, the first 5 models present NSE values between 0.5 to 0.6, CCP, and CCS of 0.8. The models slightly overestimate temperature and underestimate precipitation. The models with the best ability were CIESM for temperature and the IPSL-CM6A-LR model for precipitation. Additionally, the average of 66 local stations is compared with CRU, presenting a KGE of 0.51, CCP of 0.77 for precipitation, and NSE of -0.,17, and a CCP of 0.20 for temperature. Finally, a table is presented with the first 10 models for each variable.


Subject(s)
Rain , Seasons , Temperature , Climate Models , Climate Change/statistics & numerical data , Droughts , Guatemala , Gas Chromatography-Mass Spectrometry/methods
12.
São Paulo; s.n; s.n; 2022. 74 p. tab, graf, ilus.
Thesis in Portuguese | LILACS | ID: biblio-1396025

ABSTRACT

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 , Odorants
13.
São Paulo; s.n; s.n; 2022. 74 p. tab, graf, ilus.
Thesis in Portuguese | LILACS | ID: biblio-1391022

ABSTRACT

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/analysis
14.
Journal of Forensic Medicine ; (6): 726-732, 2022.
Article in English | WPRIM | ID: wpr-984164

ABSTRACT

OBJECTIVES@#To analyze the chemical structure of the interfering substance that affects the result of methamphetamine analysis in wastewater.@*METHODS@#A combination of GC-MS and liquid chromatography-quadrupole time-of-flight mass spectrometry (LC-QTOF-MS) was used to analyze the mass spectrum characteristics of the interfering substance that affects the result of methamphetamine analysis and to infer its possible structure. Liquid chromatography-triple quadrupole-mass spectrometry (LC-TQ-MS) was used to confirm the control material.@*RESULTS@#Using LC-QTOF-MS in positive electrospray ionization (ESI+) mode, the mass-to-charge ratio (m/z) of quasi-molecular ion in the MS1 mass spectrometry of interfering substance was identical to that of methamphetamine, indicating that the interfering substance was probably an isomer of methamphetamine. The MS2 mass spectra obtained at three collision energies of 15 V, 30 V and 45 V were highly similar to methamphetamine, suggesting that the interfering substance contained methylamino and benzyl groups. Further analysis using GC-MS in electron impact (EI) ionization mode showed that the base peak in the mass spectrum of the interfering substance was at m/z 44. The interfering substance was confirmed to be N-methyl-2-phenylpropan-1-amine by compared with the standard reference.@*CONCLUSIONS@#The chemical structure of N-methyl-2-phenylpropan-1-amine is highly similar to methamphetamine, which is easy to cause interference for the detection of trace amounts of methamphetamine in wastewater using LC-TQ-MS. Therefore, in the actual analysis, the chromatographic retention time can be used to distinguish between N-methyl-2-phenylpropan-1-amine and methamphetamine.


Subject(s)
Methamphetamine , Wastewater , Amines , Gas Chromatography-Mass Spectrometry/methods , Mass Spectrometry/methods , Spectrometry, Mass, Electrospray Ionization/methods
15.
Journal of Forensic Medicine ; (6): 473-477, 2022.
Article in English | WPRIM | ID: wpr-984138

ABSTRACT

OBJECTIVES@#To establish a method to identify unknown sample based on the combined use of Fourier transform infrared spectroscopy (FTIR), gas chromatography-quadrupole time-of-flight mass spectrometry (GC-QTOF-MS), ultra-high performance liquid chromatography-linear ion trap quadrupole-orbitrap mass spectrometry (UPLC-LTQ-Orbitrap MS) and 1H-nuclear magnetic resonance spectroscopy (1H-NMR) technique.@*METHODS@#The unknown sample was directly analyzed by FTIR. The unknown sample was dissolved in methanol solution containing internal standard SKF525A and the supernatant was detected by GC-QTOF-MS and UPLC-LTQ-Orbitrap MS. The unknown sample was dissolved in methanol-d4 solution for structural analysis of 1H-NMR.@*RESULTS@#The characteristic absorption peaks of FTIR spectra obtained from unknown sample were 1 682 (C=O bond), 1 503, 1 488, 1 436, 1 363, 1 256, 1 092, 1 035, 935, 840 and 800 cm-1, the characteristic fragment ions (m/z) of GC-QTOF-MS were 86.096 4 (base peak), 58.065 1, 149.023 5, 121.028 6 and 65.038 6, the accurate mass [M+H]+ detected by UPLC-LTQ-Orbitrap MS was 236.127 7. The sample was identified as synthetic cathinone new psychoactive substance Eutylone by 1H-NMR.@*CONCLUSIONS@#The method established in this study can be used for structural confirmation of Eutylone.


Subject(s)
Methanol , Chromatography, High Pressure Liquid/methods , Mass Spectrometry , Gas Chromatography-Mass Spectrometry/methods , Magnetic Resonance Spectroscopy
16.
Acta bioquím. clín. latinoam ; 54(1): 61-68, mar. 2020. graf, tab
Article in Spanish | LILACS | ID: biblio-1130580

ABSTRACT

El uso de bisfenol-A (BPA) a nivel de la industria global se ha venido incrementando en los ultimos anos, y fueron los mercados emergentes los impulsores de esta demanda creciente. Las aplicaciones de BPA en la industria de los alimentos y bebidas representan solo del 3 al 4% del consumo global de policarbonato, pero su uso esta siendo reexaminado debido a que se conocieron varios trabajos cientificos que indican la existencia de una relacion directa entre el BPA y los efectos adversos para la salud. La contaminacion de los alimentos y bebidas se produce por migracion del BPA desde los envases que los contienen (alimentos enlatados, vinos, etc.), y es la principal fuente de exposicion en el humano. Para evaluar dicha exposicion se desarrollo y valido un metodo analitico por cromatografia gaseosa acoplada a espectrometria de masa para la cuantificacion de BPA total en orina de mujeres embarazadas atendidas en el Hospital Italiano de Buenos Aires en el ano 2013, con un limite de cuantificacion de 2,0 ng/mL y un limite de deteccion de 0,8 ng/mL. De las 149 muestras de orina analizadas, el 66,4% fueron cuantificables, con la mediana de BPA total de 4,8 ng/mL (4,3 ng/mg de creatinina) y la media geometrica de 4,8 ng/mL (4,7 ng/mg de creatinina).


The use of bisphenol-A (BPA) at the level of the global industry has been increasing in recent years, with emerging markets being the drivers of this growing demand. BPA applications in the food and beverage industry represent only 3 to 4% of the global consumption of polycarbonate, but its use is being reexamined because several scientific works were reported indicating the existence of a direct relationship between BPA and adverse effects on health. The contamination of food and beverages is produced by the migration of BPA from the containers that hold them (canned foods, wines, etc.) and it is the main source of exposure in humans. To evaluate this exposure, an analytical method was developed by gas chromatography coupled to mass spectrometry for the quantification of total BPA in urine of pregnant women treated at the Hospital Italiano de Buenos Aires in 2013, with a limit of quantification of 2.0 ng/mL and of detection of 0.8 ng/mL. Of the 149 urine samples analyzed, 66.4% were quantifiable, with a median total BPA of 4.8 ng/mL (4.3 ng/mg creatinine) and a geometric mean of 4.8 ng/mL (4.7 ng/mg creatinine).


O uso de bisfenol-A (BPA) ao nivel da industria global foi aumentando nos ultimos anos, e foram os mercados emergentes que deram impulso a essa demanda crescente. As aplicacoes de BPA na industria de alimentos e bebidas representam apenas 3 a 4% do consumo global de policarbonato, mas seu uso esta sendo reexaminado visto que varios trabalhos cientificos indicando a existencia de uma relacao direta entre o BPA e os efeitos adversos na saude foram conhecidos. A contaminacao dos alimentos e bebidas e produzida pela migracao de BPA das embalagens que os contem (alimentos enlatados, vinhos, etc.) e e a principal fonte de exposicao em humanos. Para avaliar esta exposicao, foi desenvolvido e avaliado um metodo analitico por cromatografia gasosa acoplada a espectrometria de massas para a quantificacao do BPA total na urina de gestantes atendidas no Hospital Italiano de Buenos Aires em 2013, com um limite de quantificacao de 2,0 ng/mL e um limite de deteccao de 0,8 ng/mL. Das 149 amostras de urina analisadas, 66,4% foram quantificaveis, com uma mediana de BPA total de 4,8 ng/mL (4,3 ng/mg de creatinina) e a media geometrica de 4,8 ng/mL (4,7 ng/mg de creatinina).


Subject(s)
Humans , Female , Pregnancy , Urine , Pregnancy/urine , Endocrine Disruptors , Gas Chromatography-Mass Spectrometry/methods , Mass Spectrometry/methods , Toxicology/statistics & numerical data , Food Industry , Health , Chromatography, Gas/methods , Food and Beverages , Pregnant Women , Drug-Related Side Effects and Adverse Reactions , Food
17.
Journal of Zhejiang University. Science. B ; (12): 172-177, 2020.
Article in English | WPRIM | ID: wpr-1010524

ABSTRACT

Blakeslea trispora is a natural source of carotenoids, including β-carotene and lycopene, which have industrial applications. Therefore, classical selective breeding techniques have been applied to generate strains with increased productivity, and microencapsulated β-carotene preparation has been used in food industry (Li et al., 2019). In B. trispora, lycopene is synthesized via the mevalonate pathway (Venkateshwaran et al., 2015). Lycopene cyclase, which is one of the key enzymes in this pathway, is a bifunctional enzyme that can catalyze the cyclization of lycopene to produce β-carotene and exhibit phytoene synthase activity (He et al., 2017).


Subject(s)
Citric Acid Cycle , Fermentation , Gas Chromatography-Mass Spectrometry/methods , Lycopene/metabolism , Mucorales/metabolism , Nicotine/pharmacology , beta Carotene/biosynthesis
18.
Braz. J. Pharm. Sci. (Online) ; 56: e18664, 2020. tab, graf
Article in English | LILACS | ID: biblio-1249153

ABSTRACT

Abstract The present study describes a method for simultaneous analysis of cocaine, benzoylecgonine and cocaethylene in urine samples. After solid phase extraction, Gas Chromatography-Mass Spectrometry was used for identification and quantification. The calibration curves were linear at 20 - 3000 ng/mL, r2 0.9997 for benzoylecgonine, 15 - 2000 ng/mL, r2 0.9985 and r2 0.9993 for cocaine and cocaethylene, respectively. Accuracy values: cocaine: 93,5 - 102,1%; benzoylecgonine: 97,5 - 104,8%; cocaethylene: 90,6 - 101,5%. Precision values: cocaine: C.V 5,4 - 14,6%; benzoylecgonine: C.V 7,8 - 12,3%; cocaethylene: C.V 5,9 - 12,3%. Detection and quantification limit values: cocaine and cocaethylene:10 ng/mL and 15 ng/mL, respectivalty; benzoylecgonine:15 ng/mL and 20 ng/mL, respectivaley. Recovery values: cocaine: 78,0 - 85,8%; benzoylecgonine: 74,0 - 79,8%; cocaethylene: 83,0 - 91,5%. The method described is advantageous compared to others, as it simultaneously detects the major analytes found in urine samples due to cocaine use and has been successfully validated.


Subject(s)
Humans , Male , Female , Urine , Cocaine/analysis , Validation Study , Gas Chromatography-Mass Spectrometry/methods , Methods
19.
Braz. J. Pharm. Sci. (Online) ; 56: e18371, 2020. tab
Article in English | LILACS | ID: biblio-1132038

ABSTRACT

This study aims to investigate chemical composition of essential oils from Murraya paniculata (L.) Jack (Rutaceae) ripe and unripe fruits and determine their in vitro antibacterial activity. Essential oils were extracted by hydrodistillation from Murraya paniculata (L.) Jack ripe and unripe fruits collected in the Cerrado, in Rio Verde, southwestern Goiás, Brazil. They were analyzed by gas chromatography with flame ionization detector (GC-FID) and by gas chromatography-mass spectrometry (GC-MS). Sesquiterpenes, which represent the most abundant class of compounds in oils, predominated in both ripe and unripe fruits. Major constituents of essential oils extracted from ripe fruits (RF-EO) were (-caryophyllene (21.3%), (-ylangene (13.3%), germacrene-D (10.9%) and (-zingiberene (9.7%) whereas the ones of unripe fruits (UF-EO) were sesquithujene (25.0%), (-zingiberene (18.2%), germacrene-D (13.1%) and (-copaene (12.7%). In vitro antibacterial activity of essential oils was evaluated in terms of its minimum inhibitory concentration (MIC) values by the broth microdilution method in 96-well microplates. Both essential oils under investigation showed moderate anti-streptococcal activity against the following bacteria: Streptococcus mutans, S. mitis, S. sanguinis, S. sobrinus and S. salivarius. MIC values ranged between 100 and 400 µg/mL. Regarding the antimycobacterial activity, essential oils from M. paniculata (L.) Jack unripe and ripe fruits were active against Mycobacterium kansasii (MIC = 250 µg/mL), moderately active against M. tuberculosis (MIC = 500 µg/mL) and inactive against M. avium (MIC = 2000 µg/mL). This study was pioneer in revealing similar chemical profiles of both essential oils extracted from Murraya paniculata (L.) Jack unripe and ripe fruits, besides describing their in vitro anti-streptococcal and antimycobacterial activities.


Subject(s)
In Vitro Techniques/methods , Oils, Volatile/chemistry , Rutaceae/anatomy & histology , Murraya/classification , Fruit/anatomy & histology , Streptococcus mutans , Microbial Sensitivity Tests , Chromatography, Gas/instrumentation , Mycobacterium kansasii , Gas Chromatography-Mass Spectrometry/methods , Mycobacterium/classification
20.
Bol. latinoam. Caribe plantas med. aromát ; 18(5): 492-503, sept. 2019. tab, ilus
Article in English | LILACS | ID: biblio-1008286

ABSTRACT

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.


Subject(s)
Hedeoma , Solid Phase Microextraction/methods , Volatile Organic Compounds/chemistry , Gas Chromatography-Mass Spectrometry/methods
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