RESUMO
The Athabasca oil sands region (AOSR) of Alberta, Canada is notable for its considerable unconventional petroleum extraction projects, where bitumen is extracted from naturally-occurring oil sands ore. The large scale of these heavy crude oil developments raises concerns because of their potential to distribute and/or otherwise influence the occurrence, behaviour, and fate of environmental contaminants. Naphthenic acids (NAs) are one such contaminant class of concern in the AOSR, so studies have examined the occurrence and molecular profiles of NAs in the region. We catalogued the spatiotemporal occurrence and characteristics of NAs in boreal wetlands in the AOSR over a 7-year period, using derivatized liquid chromatography-tandem mass spectrometry (LC-MS/MS). Comparing median concentrations of NAs across these wetlands revealed a pattern of NAs suggesting NAs in surface waters derived from oil sands deposits. Opportunistic wetlands that formed adjacent to reclaimed overburden and other reclamation activities had the highest concentrations of NAs and consistent patterns suggestive of bitumen-derived inputs. However, similar patterns in the occurrence of NAs were also observed in undeveloped natural wetlands located above the known surface-mineable oil sands deposit that underlies the region. Intra-annual sampling results along with inter-annual comparisons across wetlands demonstrated that differences in the spatial and temporal NA concentrations were dependent on local factors, particularly when naturally occurring oil sands ores were observed in the wetland or drainage catchment.
Assuntos
Petróleo , Poluentes Químicos da Água , Alberta , Campos de Petróleo e Gás , Áreas Alagadas , Cromatografia Líquida , Espectrometria de Massas em Tandem , Petróleo/análise , Ácidos Carboxílicos/análise , Poluentes Químicos da Água/análiseRESUMO
The chemical composition of root exudates and root extracts from Chrysopogon zizanioides (L.) Roberty cv KS-1 was determined in the presence of lead [Pb(II)]. Hitherto, no information is available in the literature concerning the phytochemical components of root exudates of C. zizanioides. Significantly higher concentrations of total carbohydrates (26.75 and 42.62% in root exudates and root extract, respectively), reducing sugars (21.46 and 56.11% in root exudates and root extract, respectively), total proteins (9.22 and 23.70% in root exudates and root extract, respectively), total phenolic acids (14.69 and 8.33% in root exudates and root extract, respectively), total flavonoids (14.30 and 12.28% in root exudates and root extract, respectively), and total alkaloids (12.48 and 7.96% in root exudates and root extract, respectively) were observed in samples from plants growing under Pb(II) stress in comparison to the respective controls. GC-MS profiling showed the presence of a diverse group of compounds in root exudates and extracts, including terpenes, alkaloids, flavonoids, carotenoids, plant hormones, carboxylic/organic acids, and fatty acids. Among the detected compounds, many have an important role in plant development, regulating rhizosphere microbiota and allelopathy. Furthermore, the results indicated that C. zizanioides exudates possess a chemotactic response for rhizospheric bacterial strains Bacillus licheniformis, Bacillus subtilis, and Acinetobacter junii Pb1.
Assuntos
Vetiveria , Bactérias , Ácidos Carboxílicos/análise , Vetiveria/metabolismo , Exsudatos e Transudatos , Flavonoides/farmacologia , Chumbo/análise , Compostos Fitoquímicos/farmacologia , Extratos Vegetais/farmacologia , Raízes de Plantas/metabolismoRESUMO
BACKGROUND: Pasture farming in south-western Australia is challenged by nutrient-poor soils. We assessed the impact of microbial consortium inoculant (MI) and rock mineral fertiliser (MF) on growth, nutrient uptake, root morphology, rhizosphere carboxylate exudation and mycorrhizal colonisation in three pasture grasses - tall fescue (Festuca arundinacea L.), veldt grass (Ehrharta calycina Sm.) and tall wheatgrass (Thinopyrum ponticum L.) grown in low-phosphorus (P) sandy soil in a glasshouse for 30 and 60 days after sowing (DAS). RESULTS: Veldt grass produced the highest specific root length and smallest average root diameter in both growth periods, and had similar shoot weight, root surface area and fine root length (except at 30 DAS) to tall fescue. Compared with the control, MI alone or combined with MF significantly increased shoot and root biomass (except root biomass at 30 DAS), likely due to the significant increases in root surface area and fine root length. Plants supplied with MI + MF had higher shoot N and P contents than those in the MI and the control treatments at 60 DAS. Malate, citrate and trans-aconitate were the major rhizosphere carboxylates exuded at both 30 and 60 DAS. Malate exudation varied among species and treatments in both growth periods, but citrate exudation was consistently higher in the low-P treatments (control and MI) than the MF and MI + MF treatments. CONCLUSION: Microbial consortium inoculant can positively influence pasture production in low-P soil by increasing root surface area and fine root length, whereas exudation of nutrient-mobilising carboxylates (citrate) is dependent more on soil P supply than microbial consortium inoculant. © 2021 Society of Chemical Industry.
Assuntos
Inoculantes Agrícolas/crescimento & desenvolvimento , Micorrizas/crescimento & desenvolvimento , Fósforo/análise , Exsudatos de Plantas/metabolismo , Raízes de Plantas/crescimento & desenvolvimento , Poaceae/microbiologia , Ácidos Carboxílicos/análise , Ácidos Carboxílicos/metabolismo , Fertilizantes/análise , Consórcios Microbianos , Fósforo/metabolismo , Exsudatos de Plantas/análise , Raízes de Plantas/química , Raízes de Plantas/metabolismo , Raízes de Plantas/microbiologia , Poaceae/química , Poaceae/crescimento & desenvolvimento , Poaceae/metabolismo , Rizosfera , Solo/químicaRESUMO
This work describes the surface coating of wooden toothpicks with amino groups (NH2) for electrospray ionization mass spectrometry (MS) analysis of naphthenic acids (NAs) in produced water samples and crude oil fractions. NH2 was introduced into the cellulosic material through a silanization reaction using aminopropyltriethoxysilane. An NH2-modified toothpick was inserted into the analyte extraction sample and was subsequently used as an electrospray emitter for MS analysis. The extraction conditions were optimized by analyzing NAs (benzoic acid, 1-naphthoic acid, decanoic acid, 3,5-dimethyladamantane-1-carboxylic acid, and 3,5-dimethyladamantane-1-acetic acid) in pure water, and the best condition was using 5 min of extraction time with the samples under agitation. Modified and unmodified wooden toothpicks were compared, and the intensities of all NAs were higher when using the modified substrates than when using the unmodified ones. Limit of detection (LOD), limit of quantification (LOQ), linearity, precision, and recovery were determined by analyzing decanoic acid in seawater samples. The LOD and LOQ were 2 and 5 µg mL-1, respectively, and a linear correlation (R2 = 0.9927) was obtained with concentrations ranging from 5 to 250 µg mL-1. Precision values ranged from 6 to 13% and recoveries from 89 to 106%. The technique was also employed to analyze three produced water samples, in which decanoic acid was semi-quantified, and the concentrations ranged from 10 to 13 µg mL-1. High abundances of acidic compounds of class O2 with DBEs (double bond equivalents) ranging from 1 to 3 and carbon numbers going from 8 to 12 were detected in the produced water samples. The results suggest that the modification of wooden toothpicks with NH2 might offer a significant advancement in the knowledge of cheap substrates that can improve the sensitivity of analysis of NAs in water samples.
Assuntos
Petróleo , Espectrometria de Massas por Ionização por Electrospray , Ácidos Carboxílicos/análise , Ácidos Carboxílicos/química , Espectrometria de Massas por Ionização por Electrospray/métodos , ÁguaRESUMO
Due to the health-promoting properties of elderberry fruits, which result from their rich chemical composition, this raw material is widely used in herbal medicine and the food industry. The aim of the study was to demonstrate the antibacterial activity of the elderberry fruit extracts. The research showed that the content of phenolic acids and flavonoids in the extracts determined their antibacterial activity. The research showed that the content of phenolic acids and flavonoids in the extracts determined their antibacterial activity. The following phenolic acids were predominant: chlorogenic acid, sinapic acid, and t-cinnamic acid. Their average content was, respectively, 139.09, 72.84, 51.29 mg/g extract. Rutin and quercetin (their average content was 1105.39 and 306.6 mg/g extract, respectively) were the dominant flavonoids. The research showed that the elderberry polyphenol extracts exhibited activity against selected strains of bacteria within the concentration range of 0.5-0.05%. The following bacteria were the most sensitive to the extracts: Micrococcus luteus, Proteus mirabilis, Pseudomonas fragii, and Escherichia coli. Of the compounds under analysis, apigenin, kaempferol and ferulic, protocatechuic, and p-coumarin acids had the greatest influence on the high antibacterial activity of elderberry extracts. The results of the microbiological and chemical analyses of the composition of the extracts were analyzed statistically to indicate the bioactive compounds of the greatest antimicrobial significance.
Assuntos
Anti-Infecciosos/farmacologia , Antioxidantes/farmacologia , Extratos Vegetais/farmacologia , Sambucus nigra/química , Bactérias/efeitos dos fármacos , Benzotiazóis/química , Ácidos Carboxílicos/análise , Flavonoides/análise , Testes de Sensibilidade Microbiana , Pigmentos Biológicos/análise , Polifenóis/análise , Ácidos Sulfônicos/químicaRESUMO
The prebiotic effect of high ß-glucan barley (HGB) flour on the innate immune system of high-fat model mice was investigated. C57BL/6J male mice were fed a high-fat diet supplemented with HGB flour for 90 days. Secretory immunoglobulin A (sIgA) in the cecum and serum were analyzed by enzyme-linked immunosorbent assays (ELISA). Real-time PCR was used to determine mRNA expression levels of pro- and anti-inflammatory cytokines such as interleukin (IL)-10 and IL-6 in the ileum as well as the composition of the microbiota in the cecum. Concentrations of short-chain fatty acids (SCFAs) and organic acids were analyzed by GC/MS. Concentrations of sIgA in the cecum and serum were increased in the HGB group compared to the control. Gene expression levels of IL-10 and polymeric immunoglobulin receptor (pIgR) significantly increased in the HGB group. HGB intake increased the bacterial count of microbiota, such as Bifidobacterium and Lactobacillus. Concentrations of propionate and lactate in the cecum were increased in the HGB group, and a positive correlation was found between these organic acids and the IL-10 expression level. Our findings showed that HGB flour enhanced immune function such as IgA secretion and IL-10 expression, even when the immune system was deteriorated by a high-fat diet. Moreover, we found that HGB flour modulated the gut microbiota, which increased the concentration of SCFAs, thereby stimulating the immune system.
Assuntos
Ceco/imunologia , Farinha , Hordeum , Íleo/imunologia , Obesidade/imunologia , Prebióticos , beta-Glucanas/análise , Animais , Carga Bacteriana , Peso Corporal , Ácidos Carboxílicos/análise , Ceco/química , Ceco/microbiologia , Citocinas/genética , Citocinas/metabolismo , Dieta , Ingestão de Alimentos , Ácidos Graxos Voláteis/análise , Fezes/química , Microbioma Gastrointestinal , Perfilação da Expressão Gênica , Íleo/metabolismo , Imunoglobulina A Secretora/análise , Imunoglobulina A Secretora/sangue , Masculino , Camundongos , Camundongos Endogâmicos C57BL , Tamanho do Órgão , RNA Mensageiro/genética , RNA Mensageiro/metabolismo , Receptores de Imunoglobulina Polimérica/genética , Receptores de Imunoglobulina Polimérica/metabolismoRESUMO
Small white apricot is well known as a famous fresh fruit and even a folk medicine in Xinjiang. To investigate nutritive value, antioxidant activity, and flavor of small white apricot, sugars, organic acids, total flavonoids, phenolic compounds, antioxidant activities, and volatile compounds in five apricot cultivars were examined by high-performance liquid chromatography (HPLC) and headspace solid-phase microextraction coupled with gas chromatography-mass spectrometry (HS-SPME-GC-MS). The results showed that sucrose (32.94% to 42.49%), malic acid (69.21% to 76.75%), and quercetin-3-rutinoside (72.84% to 74.05%) were the dominant sugar, organic acid, and phenolic compounds in small white apricot, respectively. The antioxidant activity reached up to 61.72 to 135.52 mg TEs 100 g-1 . Furthermore, the aroma fingerprint of the small white apricot consisted of 1-octen-3-ol, 1-dodecanol, pentanal, hexanal, (E)-2-hexenal, (E)-2-heptenal, 6-methyl-5-hepten-2-one, (E)-2-nonenal, 1-octen-3-one, ß-myrcene, and linalool, providing clear green, grassy, and fatty notes. Apricots from different cultivars possessed a similar flavor, while linalool and (E)-2-hexenal had been identified as the characteristic aroma compounds in small white apricot. The results provide a complete chemical characterization of the taste, functional ingredients and aroma of the small white apricot. PRACTICAL APPLICATION: The nutritive value, antioxidant activity and flavor of small white apricot were investigated in this study. The results will provide a theoretical basis for developing characteristic variety aroma, nutritive value, and medicinal value of small white apricot.
Assuntos
Antioxidantes/análise , Ácidos Carboxílicos/análise , Frutas/química , Odorantes/análise , Fenóis/análise , Prunus armeniaca/química , Açúcares/análise , Aldeídos/análise , China , Flavonoides/análise , Frutas/crescimento & desenvolvimento , Cromatografia Gasosa-Espectrometria de Massas/métodos , Prunus armeniaca/crescimento & desenvolvimento , Microextração em Fase Sólida/métodos , Paladar , Compostos Orgânicos Voláteis/análiseRESUMO
The beneficial health properties of organic acids make them target compounds in multiple studies. This is the reason why developing a simple and sensitive determination and investigation method of organic acids is a priority. In this study, an effective method has been established for the determination of organic (lactic, glycolic, and malic) acids in saffron stigmas. N-(tert-butyldimethylsilyl)-N-methyltrifluoroacetamide (MTBSTFA) was used as a derivatization reagent in gas chromatography combined with mass spectrometric detection (GC/MS). The saffron stigmas extract was evaporated to dryness with a stream of nitrogen gas. The derivatization procedure: 0.1 g of dried extract was diluted into 0.1 mL of tetrahydrofuran, then 0.1 mL MTBSTFA was orderly and successively added into a vial. Two different techniques were used to obtain the highest amount of organic acid derivatives from saffron stigmas. To the best of our knowledge, this is the first report of the quantitative and qualitative GC/MS detection of organic acids in saffron stigmas using MTBSTFA reagent, also comparing different derivatization conditions, such as time, temperature and the effect of reagent amount on derivatization process. The identification of these derivatives was performed via GC-electron impact ionization mass spectrometry in positive-ion detection mode. Under optimal conditions, excellent linearity for all organic acids was obtained with determination coefficients of R2 > 0.9955. The detection limits (LODs) and quantitation limits (LOQs) ranged from 0.317 to 0.410 µg/mL and 0.085 to 1.53 µg/mL, respectively. The results showed that the highest yield of organic acids was conducted by using 0.1 mL of MTBSTFA and derivatization method with a conventional heating process at 130 °C for 90 min. This method has been successfully applied to the quantitative analysis of organic acids in saffron stigmas.
Assuntos
Ácidos Carboxílicos/análise , Crocus/química , Flores/química , Cromatografia Gasosa-Espectrometria de Massas , Extratos Vegetais/químicaRESUMO
Volatile and non-volatile compounds in coffee directly affect the beverage's quality. This study aimed to demonstrate how the organic acids and volatile profiles were impacted by coffee fermentation using four starter cultures (Meyerozyma caribbica (CCMA 0198), Saccharomyces cerevisiae (CCMA 0543), Candida parapsilosis (CCMA0544), and Torulaspora delbrueckii (CCMA 0684)) inoculated in two varieties of coffee (Bourbon Amarelo and Canário Amarelo) using natural and pulped natural processing methods and sensory perception. Real-time PCR (qPCR) was used to verify the dynamic behavior of yeast populations. Organic acids were detected using high performance liquid chromatography (HPLC) and gas chromatography-mass spectrometry (GC-MS) was used to detected volatile compounds. Sensory analysis was performed on the roasted coffee. Citric, malic, succinic, lactic, oxalic, isobutyric, and propionic acids and 105 volatile compounds were detected. At the beginning of fermentation, treatments with natural processing presented higher number of volatiles compounds. After fermentation, the main compounds groups were acids, alcohols, and aldehydes. The perception of sensory attribute (fruity, nutty, cocoa) varied with the coffee variety, type of processing, and type of inoculum. The use of yeasts is an alternative for sensorial differentiation of coffee variety Canário Amarelo and Bourbon Amarelo. The stainless-steel containers showed good results for coffee fermentation.
Assuntos
Ácidos Carboxílicos/análise , Café/química , Fermentação , Manipulação de Alimentos/métodos , Qualidade dos Alimentos , Fermento Seco/metabolismo , Candida parapsilosis , Ácidos Carboxílicos/química , Cromatografia Líquida de Alta Pressão , Cromatografia Gasosa-Espectrometria de Massas , Humanos , Reação em Cadeia da Polimerase , Saccharomyces cerevisiae , Saccharomycetales , TorulasporaRESUMO
In this study we explore the effects of multi-colour LED lighting spectrum on nutritive primary metabolites in green ('Lobjoits green cos') and red ('Red cos') leaf lettuce (Lactuca sativa L.), cultivated in controlled environment. The basal lighting, consisting of blue 455â¯nm, red 627 and 660â¯nm and far red 735â¯nm LEDs, was supplemented with UV-A 380â¯nm, green 510â¯nm, yellow 595â¯nm or orange 622â¯nm LED wavelengths at total photosynthetic photon flux density of 300⯵molâ¯m-2â¯s-1. Supplemental lighting colours did not affect lettuce growth; however had distinct impact on nitrite, amino acid, organic acid, and soluble sugar contents. Orange, green and UV-A light had differential effects on red and green leaf lettuce metabolism and interplay with nutritional value and safety of lettuce production. The metabolic response was cultivar specific; however green light had reasonable impact on the contents of nutritive primary metabolites in red and green leaf lettuce.
Assuntos
Aminoácidos/metabolismo , Ácidos Carboxílicos/metabolismo , Lactuca/química , Lactuca/fisiologia , Nitratos/metabolismo , Aminoácidos/análise , Ácidos Carboxílicos/análise , Ambiente Controlado , Iluminação , Nitratos/análise , Nitritos/metabolismo , Fotossíntese , Pigmentação , Açúcares/análise , Açúcares/metabolismo , Raios UltravioletaRESUMO
The promising features of fluorescence spectroscopy have inspired a quest for fluorescent probes for analysis and monitoring of molecular interactions in biochemical, medical, and environmental sciences. To overcome the competitive supramolecular interactions in aqueous media encountered with conventional molecular-recognition-based probes, the use of reaction-based probes that involve making or breaking of covalent bonds has emerged as a complementary sensing strategy to realize higher selectivity and sensitivity with larger spectroscopic changes. In spite of the enormous efforts, the development of reaction-based fluorescent probes meets with certain challenges in terms of their practical applications, demanding "intelligent design" of probes with an appropriate fluorophore attached to an efficient reactive moiety at the right place. This Account summarizes the results of our efforts made in the development and fine-tuning of reaction-based fluorescent probes toward those goals, classified by the type of analyte (anions, metal cations, and biomolecules) with notes on the challenges and achievements. The reaction-based approach was demonstrated to be powerful for the selective sensing of anions (cyanide and (amino)carboxylates) for the first time, and later it was extended to develop two-photon probes for bisulfite and fluoride ions. The reaction-based approach also enabled selective sensing of noble metal ions such as silver, gold, and palladium along with toxic (methyl)mercury species and paramagnetic copper ions. Furthermore, microscopic imaging and monitoring of biologically relevant species with reaction-based two-photon probes were explored for hydrogen sulfide, hypochlorous acid, formaldehyde, monoamine oxidase enzyme, and ATP.
Assuntos
Corantes Fluorescentes/química , Trifosfato de Adenosina/análise , Ácidos Carboxílicos/análise , Cianetos/análise , Formaldeído/análise , Sulfeto de Hidrogênio/análise , Ácido Hipocloroso/análise , Metais Pesados/análise , Monoaminoxidase/análise , Monoaminoxidase/metabolismo , Espectrometria de FluorescênciaRESUMO
In this work, the profiles of phenolics, fiber, pectins, sugars, organic acids and carotenoids, vitamin C, ash, protein and fat contents, as well as antioxidant capacity were compared in fruits, flowers, and bark of Viburnum opulus (VO). Antioxidant capacity was evaluated against ABTS, hydroxyl, peroxyl and superoxide free radicals, and as a reducing power by using in vitro test. The results showed great quantitative differences in the composition of the VO morphological parts tested. Fruits contained the highest concentrations of fat, organic acids, sugars, soluble dietary fiber (10.57 ± 0.54; 7.34 ± 0.06; 32.27 ± 1.25; 6.82 ± 0.38 g/100 g DW, respectively) and carotenoids (2.70 ± 0.07 mg/100 g DW). Whereas, the bark exceeded the remaining parts of the VO in terms of antioxidant capacity, ash (9.32 ± 0.17 g/100 g DW), total (59.34 ± 0.75 g/100 g DW) and insoluble dietary fiber (58.20 ± 0.73 g/100 g DW) contents as well as phenolic compounds (3.98 ± 0.04 g/100 g DW). Among the phenolic compounds quantified in this study, chlorogenic acid and (+)-catechin had the highest concentrations (> 1 g/100 g DW) in the flowers and bark, respectively.
Assuntos
Antioxidantes/análise , Carotenoides/análise , Nutrientes/análise , Fenóis/análise , Viburnum/química , Ácidos Carboxílicos/análise , Catequina/análise , Ácido Clorogênico/análise , Fibras na Dieta/análise , Flores/química , Frutas/química , Especificidade de Órgãos , Pectinas/análise , Casca de Planta/química , Açúcares/análiseRESUMO
Gas-chromatography (GC) analysis of carboxylic acids is limited by the high polarity and low volatility of most of these compounds. Boron trifluoride (BF3) mediated alkylation reactions is one of the most commonly used derivatization methods for making carboxylic acids GC compatible. A semi-automated BF3·EtOH (ethanol) derivatization method was optimized for comprehensive two-dimensional gas chromatography high-resolution mass spectrometry (GC × GC-HR MS) analysis of carboxylic acids in solid phase extraction (SPE) extracts of oil polluted water. The optimal derivatization method were found to be with addition of 300 µL BF3·EtOH per 200 µL sample and reaction at 75 °C for 24 h. Derivatives of eight selected acids (aliphatic, mono- and di-aromatic) were stable over 12 h with relative standard deviations (RSDs) of 2.0-10.7 %, the derivatization method was repeatable (RSDs of 3.2-17.2 %), detection limits (DL) and limit of detections (LODs) was in the range of DL = 0.53-1.63 ppb and LOD = 0.19-2.51 ppb for pure acid standards, and DL = 0.18-3.41 ppb and LOD = 0.28-5.46 ppb for matrix matched acid standards. Finally, the method was validated on the acidic fraction of a mixed anion-exchange SPE of oil polluted water. Thousands of degradation products from parent alkylated polycyclic aromatic hydrocarbons (PAHs) and aliphatic hydrocarbons, such as aliphatic acids and mono-, di- and tri- aromatic acids were analyzed by the applied method and compound groups were tentatively identified.
Assuntos
Boranos/química , Ácidos Carboxílicos/análise , Monitoramento Ambiental/métodos , Etanol/química , Água/química , Alquilação , Cromatografia Gasosa-Espectrometria de Massas , Limite de Detecção , Petróleo/análise , Hidrocarbonetos Policíclicos Aromáticos/análise , Extração em Fase Sólida , Poluentes Químicos da Água/análiseRESUMO
Pig feces is an interesting biological sample to be implemented in metabolomics experiments by virtue of the information that can be deduced from the interaction between host and microbiome. However, pig fecal samples have received scant attention, especially in untargeted metabolomic studies. In this research, an analytical strategy was planned to maximize the identification coverage of metabolites found in pig fecal samples. For this purpose, two complementary platforms such as LC-QTOF MS/MS and GC-TOF/MS were used. Concerning sample preparation six extractant solvents with different polarity grade were tested to evaluate the extraction performance and, in the particular case of GC-MS, two derivatization protocols were compared. A total number of 303 compounds by combination of all the extractants and analytical platforms were tentatively identified. The main identified families were amino acids, fatty acids and derivatives, carbohydrates and carboxylic acids. For GC-TOF/MS analysis, the recommended extractant is methanol, while methoxymation was required in the derivatization protocol since this step allows detecting the α-keto acids, which are direct markers of the microbiome status. Concerning LC-QTOF MS/MS analysis, a dual extraction approach with methanol (MeOH) or MeOH/water and ethyl acetate is proposed to enhance the detection of polar and non-polar metabolites.
Assuntos
Aminoácidos/análise , Ácidos Carboxílicos/análise , Ácidos Graxos/análise , Fezes/química , Aminoácidos/metabolismo , Animais , Ácidos Carboxílicos/metabolismo , Cromatografia Líquida , Ácidos Graxos/metabolismo , Espectrometria de Massas , SuínosRESUMO
Triacyl-, diacyl- and monoacylglycerols (TAGs, DAGs, MAGs) along with monocarboxylic acids (MCAs) are intermediate products in many triacylglycerol oil-to-biofuel conversion pathways. Accumulation of these compounds leads to poor biofuel characteristics and may result in fuel system damage. We developed a method for simultaneous identification and quantification of a wide range of MCAs (C4-C18), MAGs, DAGs, and TAGs. The method is based on trimethylsilylation followed by high temperature GC with programmed temperature vaporizer (PTV) injection coupled to parallel FID and MS detectors (HTGC-FID/MS). To minimize the discrimination of both low and high molecular weight species typically occurring on the injector, we optimized injection conditions using a central composite design. The critical variables were the time at initial temperature (40 °C), splitless time, and the interaction between these two parameters. Among three tested electron ionization source/quadrupole analyzer temperatures, a 350/200 °C setting provided the highest response and signal-to-noise ratio for TAGs and did not have an effect on MAGs and DAGs. Similar results were obtained when quantifying target analytes in intermediate products of soybean oil cracking with FID and MS (using specific acylglycerol fragmentation ions). The instrumental FID limits of detection (LODs) were 0.07-0.27 ng for most of the target analytes. Selected ion monitoring (SIM) LODs were 0.01-0.05 ng for MCAs and 0.03-0.14 ng for acylglycerols. For the total ion current (TIC), LODs observed increased with acyl chain length and degree of unsaturation, resulting in an increase from 0.05 to 0.18 ng for MCAs (C5 to C18) and from 0.03 to 1.8 ng for acylglycerols (TAGs C8 to C22). Deviations in the repeatability of sample preparation, intra- and inter-day analyses, including sample stability over an eight-day time period, did not exceed 10% variance. These results demonstrate that the developed method is accurate and robust for the determination of acylglycerols and MCAs produced during the processing of TAGs into biofuels.
Assuntos
Biocombustíveis/análise , Ácidos Carboxílicos/análise , Ionização de Chama/métodos , Cromatografia Gasosa-Espectrometria de Massas/métodos , Glicerídeos/análise , Temperatura Alta , Limite de Detecção , Óleo de Soja/químicaRESUMO
Nettle (Urtica dioica L.), tansy (Tanacetum vulgare L.), bladder campion (Silene vulgaris (Moench) Garcke, waterpepper (Polygonum hydropiper L.), common centaury (Centaurium erythraea Pers.) and rose hip fruit (Rosa canina L. cv. Plovdiv 1) were used for preparation of different water extracts (infusion, decoction and microwave extract) and ethanol (tincture) extracts. Carotenoids (lutein, lycopene and ß-carotene), tocopherols (α-, γ- and δ-), organic acids (ascorbic, malic, fumaric and citric), five macro- and three microelements, sugars and uronic acids content in the obtained extracts were analyzed. Among the investigated plants, stinging nettle, bladder campion and rose hip fruit were evaluated as most potential with respect to bioactive compounds and microelements. The results showed that the selected six medicinal plants and their extracts can be presented as sources of dietary fibers and micronutrients, which may encourage further application as food supplements and beverages as well as to motivate plant use as a dietary alternative in different foods. The present study is a first detailed analysis with respect to sugar content of decoction, infusion and tincture of S. vulgaris.
Assuntos
Carboidratos/análise , Ácidos Carboxílicos/análise , Carotenoides/análise , Magnoliopsida/química , Minerais/análise , Extratos Vegetais/química , Tocoferóis/análise , Plantas Medicinais/químicaRESUMO
Background: There are a substantial number of papers in the scientific literature reporting on the chemical composition of the Aloe vera plant. None of these investigations are truly comprehensive nor address the differences in composition that occur through processing variations in fresh leaves and commercially available product forms. Objectives: This work was to analytically examine a range of these forms and compile the findings. Methods: Fresh A. vera leaves and a number of commercial aloe juice powders were investigated for their major chemical constituents. Samples included fresh leaves from China and Mexico, plus commercial powders from different manufacturers made from different plant parts and/or manufacturing processes. The test results include moisture, ash, fiber, protein, lipids, minerals, organic acids, free sugars, and polysaccharides. The analytical methods employed comprise inductively coupled plasma-optical emission spectroscopy for minerals, high-performance anion-exchange chromatography equipped with pulsed amperometric detection for free sugars, HPLC for organic acids, and size exclusion chromatography (SEC)-multi-angle laser light scattering (MALS)-differential refractive index (dRI) for polysaccharide analyses. The absolute MW and MW distribution were determined using MALS measurement. Results: The major constituents of A. vera fresh leaf are fibers, proteins, organic acids, minerals, monosaccharides, and polysaccharides, which accounted for 85-95% of the total composition determined. In the commercial powdered aloe juice samples, four major components-organic acids, minerals, monosaccharides, and polysaccharides-accounted for 78-84% of the total composition. Apart from the four major components, products manufactured by ethanol precipitation contained high amounts of fiber and protein, while the free sugars were removed. In ethanol-precipitated products, the polysaccharide MW was less affected by manufacturing conditions and the concentration of aloe polysaccharides was higher than in products made in the nonethanol manufacturing processes. The overall chemical profiles were found to be consistent, except for the MW and content of polysaccharides in the commercial aloe samples analyzed, which were largely dependent on the types of manufacturing processes employed. Conclusions: This present study provides a comprehensive investigation of the major chemical composition of A. vera leaf and commercially derived products. The use of the SEC combined with MALS and differential RI detectors has proved to be an improved tool for the accurate determination of polysaccharide MW and contents of the various commercially available A. vera products in this study.
Assuntos
Aloe/química , Extratos Vegetais/análise , Folhas de Planta/química , Pós/análise , Ácidos Carboxílicos/análise , Ácidos Carboxílicos/isolamento & purificação , Cromatografia em Gel , Lipídeos/análise , Lipídeos/isolamento & purificação , Extratos Vegetais/isolamento & purificação , Polissacarídeos/análise , Polissacarídeos/isolamento & purificação , Proteínas/análise , Proteínas/isolamento & purificação , Refratometria , Espalhamento de Radiação , Açúcares/análise , Açúcares/isolamento & purificaçãoRESUMO
Interest in new sources of anti-inflammatory and antioxidant compounds has recently become a major research issue, with the cornelian cherry (Cornus mas L.) receiving particular attention for its significant amounts of phenolic compounds and vitamins, which exhibit a wide range of biological and pharmacological properties. This study was aimed at increasing knowledge regarding the cornelian cherry in Italy through the analysis of biologically active substances in the locally available genotype "Chieri". Spectrophotometric methods were applied to evaluate antioxidant activity, total anthocyanin content and total polyphenolic content. Identification and quantification of the main phytochemical compounds (polyphenols, monoterpenes, organic acids and vitamin C) was performed via high performance liquid chromatography coupled to a diode array detector. C. mas extracts showed high levels of total soluble solids and low acidity. High amounts of phenolic secondary metabolites were observed, with particular reference to anthocyanins (134.71 mgC3G/100 gFW), which confer remarkable nutraceutical properties to the analysed samples. These results highlight the potential of C. mas fruits as a good source of natural antioxidants, suggesting their use as a functional food. Future studies should focus on identifying other specific phytochemical compounds and the genetic traits of local varieties in order to improve cornelian cherry cultivars for food and medicine production.
Assuntos
Antocianinas/análise , Antioxidantes/análise , Cornus/química , Suplementos Nutricionais/análise , Compostos Fitoquímicos/análise , Ácido Ascórbico/análise , Ácidos Carboxílicos/análise , Fenômenos Químicos , Frutas/química , Promoção da Saúde , Itália , Monoterpenos/análise , Polifenóis/análiseRESUMO
Garlic (Allium sativum L.) is an important vegetable crop throughout the world. In Greece there are many areas which have specialized in garlic cultivation through the last decades, considered the main production areas. However, despite the significance of garlic as a food product and the high annual income of this crop, there is a decreasing trend in total cultivated area in Greece, and the local landraces are gradually neglected in favor of new imported genotypes. In the present study, garlic genotypes (local landraces/varieties, imported genotypes, commercial cultivars) from the main production regions of Greece were assessed for their chemical composition and quality (total soluble solids, dry matter content, nutritional value, mineral composition, organic acids, fatty acids content and free sugars content), and bulb morphology. The results of the present study showed significant diversity in quality features and bulb morphology, not only between the genotypes from different growing regions, but also between those of the same region. This result is interesting since it could be implemented for further improvement and valorization of this important vegetable crop through extensive breeding programs within the framework of sustainability and genetic, material conservation.
Assuntos
Alho/química , Alho/genética , Genótipo , Melhoramento Vegetal/métodos , Aminoácidos/análise , Aminoácidos/metabolismo , Antioxidantes/análise , Antioxidantes/metabolismo , Ácidos Carboxílicos/análise , Ácidos Carboxílicos/metabolismo , Ácidos Graxos/análise , Ácidos Graxos/metabolismo , Alho/anatomia & histologia , Alho/classificação , Variação Genética , Grécia , Minerais/análise , Minerais/metabolismo , Valor Nutritivo , Proteínas de Plantas/análise , Proteínas de Plantas/metabolismo , Açúcares/análise , Açúcares/metabolismoRESUMO
Wild edible mushrooms are considered as a cheap food source, but rich in bioactive compounds, especially in phenolic compounds. The purpose of the study was to determine the antioxidant and antimicrobial activity and the content of polyphenolcarboxylic acids in 10 species of mushrooms commonly used (consumed) in Romania and two controls. The effect against free radicals, lipid peroxidation and reducing power were determined. The antimicrobial effect was revealed on some strains with pathogenic effect by disk diffusion assay. The antioxidant capacity expressed in vitro was correlated both with the presence of the main polyphenolcarboxylic acids, and also with the presence of other bioactive molecules (flavonoids, carotenoid compounds, etc.).