Cerrato, AndreaPiovesana, SusyAita, Sara ElsaCavaliere, Chiara...
10页
查看更多>>摘要：Introduction Blueberries are known for their very high content of biologically active phenolic compounds; nonetheless, differently from the North American and European species of blueberries, Neotropical blueberries have not been extensively studied yet. Objectives In the present paper, the phenolic composition of Vaccinium floribundum Kunth, which is endemic to the Andean regions and grows 1,600 to 4,500 meters above sea level, was investigated by ultra-high-performance liquid chromatography coupled to high-resolution mass spectrometry (UHPLC-HRMS). Native and fermented berries were compared in terms of phenolic composition as well as antioxidant activity, total phenolic content, and total anthocyanin content. Materials and Methods V. floribundum native and fermented berries were extracted and analyzed by UHPLC-HRMS. The acquired datasets were processed by Compound Discoverer 3.1 using a dedicated data analysis workflow that was specifically set up for phenolic compound identification. Results In total, 309 compounds were tentatively identified, including anthocyanins, flavonoids, phenolic acids, and proanthocyanidins. The molecular transformations of phenolic compounds during fermentation were comprehensively investigated for the first time, and by a customized data processing workflow, 13 quinones and quinone methides were tentatively identified in the fermented samples. Compared to other species of the genus Vaccinium, a peculiar phenolic profile is observed, with low abundance of highly methylated compounds. Conclusion Andean berries are a rich source of a wide variety of phenolic compounds. Untargeted MS analyses coupled to a dedicated data processing workflow allowed expanding the current knowledge on these berries, improving our understanding of the fate of phenolic compounds after fermentation.
查看更多>>摘要：Introduction: The diterpenoids are the most important active constituents that contribute to the pharmacological efficacy of Isodon serra (Maxim.) Hara. Clinical studies have revealed that diterpenoids possess multiple features, e.g. antitumour, antitubercular and anti-ischemic activities. Therefore, the identification and detection of diterpenoids may be equally important for understanding the pharmacological basis of diterpenoids and enhancing the product quality control of I. serra. Objectives: The purpose of this study was to develop a practical analysis approach of rapid characterisation using ultrahigh-performance liquid chromatography quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) for the structure characterisation of the ent-kaurane diterpenoids from I. serra. Methodology: The analytical strategy was as follows: first, ent-kaurane diterpenoids were detected by a novel on-line data acquisition approach, i.e. sequential window acquisition of all theoretical fragment-ion spectra (SWATH). Second, the MS of eight ent-kaurane diterpenoids was explored, and their mass spectrum cleavage pathways were summarised and determined. Finally, the methanol extract of I. serra was studied using SWATH and identified by extracted ion chromatography (XIC). Results: Compared to the traditional information-dependent acquisition (IDA) method, SWATH significantly improved the hit rate of ent-kaurane diterpenoids. With support from UHPLC separation and specific detection by tandem mass spectrometry (MS/MS), 48 ent-kaurane diterpenoids were successfully characterised and classified as ent-kaurane diterpenoids from a complex matrix. Conclusions: These combined qualitative methods were used to provide a potential approach for the characterisation of traditional Chinese medicine (TCM) and its preparations. Meanwhile, the SWATH provided a novel and reliable method for the structural characterisation of ent-kaurane diterpenoids from other complicated TCMs.
Borges, Ricardo MoreiraMendes Resende, Joao VictorPinto, Acucena PucuGarrido, Bruno Carius...
10页
查看更多>>摘要：Introduction In this era of 'omics' technology in natural products studies, the complementary aspects of mass spectrometry (MS)- and nuclear magnetic resonance (NMR)-based techniques must be taken into consideration. The advantages of using both analytical platforms are reflected in a higher confidence of results especially when using replicated samples where correlation approaches can be used to statistically link results from MS to NMR. Objectives Demonstrate the use of Statistical Total Correlation (STOCSY) for linking results from MS and NMR data to reach higher confidence in compound identification. Methodology Essential oil samples of Melaleuca alternifolia and M. rhaphiophylla (Myrtaceae) were used as test objects. Aliquots of 10 samples were collected for GC-MS and NMR data acquisition [proton (H-1)-NMR, and carbon-13 (C-13)-NMR as well as two-dimensional (2D) heteronuclear single quantum correlation (HSQC), heteronuclear multiple-bond correlation (HMBC), and HSQC-total correlated spectroscopy (TOCSY) NMR]. The processed data was imported to Matlab where STOCSY was applied. Results STOCSY calculations led to the confirmation of the four main constituents of the sample-set. The identification of each was accomplished using; MS spectra, retention time comparison, C-13-NMR data, and scalar correlations of the 2D NMR spectra. Conclusion This study provides a pipeline for high confidence in compound identification using a set of essential oils samples as test objects for demonstration.
查看更多>>摘要：Introduction Folium nelumbinis is used as vegetable, functional food and herbal medicine in Asia. p-Sulfonatocalix[6]arene (SC6A) is a water-soluble supramolecular macrocycle and has never been applied to the extraction of herbal products. Objective In this study, SC6A-assisted extraction of nuciferine from Folium nelumbinis has been carried out to develop an eco-friendly extraction process with high extraction efficacy and easy operation. Methods Single-factor experiments were adopted to obtain the optimal conditions for the SC6A-assisted extraction of nuciferine from Folium nelumbinis, and then nuciferine and SC6A were separated easily by one-step alkalization. The host-guest complexes between nuciferine and SC6A were analyzed by competitive fluorescence titration, DSC, FT-IR and H-1-NMR. Results The optimal SC6A/Folium nelumbinis/solution ratio for extraction was 0.4:1:20 (g/g/mL), with a granulometric fraction below 180 mu m and an extraction time of 1 h with soaking. The purity and recovery of nuciferine extracted with SC6A were increased 29.24 and 35.73 times compared with extraction with aqueous solution, respectively. Moreover, a good reusability of SC6A in the extraction of nuciferine was demonstrated. Competitive fluorescence titration, DSC, FT-IR and H-1-NMR characterization indicated that SC6A could form host-guest complexes with nuciferine at a ratio of 1:1. Conclusion The study provided an eco-friendly, safe and effective nuciferine extraction method, which can be used for the development of nutrition supplements containing nuciferine.
查看更多>>摘要：Introduction Food industry generates large amounts of waste by-products rich in natural antioxidants. On the other hand, application of advanced processes for the recovery of these fine chemicals is another popular topic of recent years. Objective The purpose of this study is to propose a green extraction method by application of deep eutectic solvent-based automated solvent extraction (AMSE) from lemon peels. Methods The primary polyphenols (hesperidin, naringin, and p-coumaric acid) and the total polyphenols of the lemon peel extract were quantified and used as response for the optimisation of the AMSE conditions. The Box-Behnken design type of the response surface method (RSM) was chosen for optimisation study. Scavenging activity of the lemon peel extract against 2,2-diphenyl-1-picrylhydrazil (DPPH) free radical was also measured in vitro. Results The optimum conditions for the highest total phenolic (7.47 mg-gallic acid equivalent [GAE]/g-lemon peel [LP]), naringin (5.05 mg/g-LP), p-coumaric acid (3.27 mg/g-LP), and hesperidin (0.07 mg/g-LP) yields were obtained by 1.5 h of extraction time, 46% water (v/v), and 5 g of peel. The antioxidant activity changed between 37.31% and 94.10% in the peels. Conclusions Extraction time was the most effective process factor for the total phenolic and p-coumaric acid yields, while water addition was statistically very important (p < 0.0001) for the naringin and hesperidin yields in the current AMSE system. The second-order models generated for the selected systems represent the data satisfyingly based on the high coefficients of determination (> 0.99), statistically significant p-values (<0.0001), coefficient of variation values (< 10%), and non-significant lack-of-fit values (p > 0.05).
Ockun, Mehmet AliGercek, Yusuf CanDemirsoy, HusnuDemirsoy, Leyla...
13页
查看更多>>摘要：Introduction Sweet cherry (Prunus avium L.), one of the most consumed fruits in the world, is rich in phenolic and especially anthocyanin content. Objective The aim of this study was to evaluate the phenolic properties of 11 different sweet cherry genotypes collected from Giresun, Turkey. Methods Total phenol, flavonoid, anthocyanin and antioxidant properties were observed spectrophotometrically in three different extraction (conventional, microwave-assisted and ultrasound-assisted) processes. Major phenolic, anthocyanin and antioxidant structures were visually assessed by high-performance thin layer chromatography (HPTLC). Various phenolics in its structure were determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Results T2 and E5 genotypes had the highest content in terms of total phenol, flavonoid, anthocyanin and antioxidant activity. In HPTLC, cherry samples contained high levels of chlorogenic acid, neochlorogenic acid, p-coumaroylquinic acid, rutin and cyanidin-3 rutinoside. Among the phenolics examined in the LC-MS/MS method, the major compounds in the structure of cherry were found to be chlorogenic acid, rutin and catechin. The T2 genotype had higher phenolics than the other cherry samples (chlorogenic acid 19.3 mg/100 g; catechin; 3.8 mg/100 g; rutin 33.1 mg/100 g). Conclusion As a result, T2 and E5 genotypes had higher phenolic and antioxidant activity compared to other genotypes and commercial cultivars. It can be said that the antioxidant contents of these genotypes are due to the high anthocyanin amount in their structures. In addition, T2 genotype contained more major phenolics than other cherries. In the next stage, it is recommended to carry out studies on the cultivation of these two varieties.
查看更多>>摘要：Aim To establish a fast, sensitive and accurate high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method for determining the monosaccharide content of Qingzhuan Dark Tea polysaccharides in different years (2 years, 5 years and 11 years). Methods The optimised chromatographic conditions were achieved on a C18 column (5.0 mu m, 250 mm x 4.6 mm inner diameter). The mobile phase flow rate was 0.9 mL/min and the column temperature was set to 27 degrees C. The aqueous phase A (5 mM aqueous ammonium acetate) and organic phase B (acetonitrile) were used to elute the target analyses isocratically (0-60 min: 18% B). The mass spectrometer detector was equipped with an electron spray ionisation (ESI)source, and multiple reaction monitoring (MRM) mode was used for the determination of 1-phenyl-3-methyl-5-pyrazolone (PMP) derived monosaccharides. Results We carried out a comprehensive methodological validation of PMP derived monosaccharides, including linearity, precision, stability and repeatability. Nine monosaccharides (rhamnose, mannose, ribose, glucose, galacturonic acid, xylose, galactose, fucose and arabinose) of Qingzhuan Dark Tea polysaccharides were identified, in which ribose and fucose were reported for the first time. The results showed the contents of these nine monosaccharides differed significantly among different years. Conclusions The validated method is reliable, accurate, repeatable and can be applied to quality assessment of these monosaccharides.
查看更多>>摘要：Introduction The quantitative analysis of trace resveratrol and polydatin in plant tissues is suitable for elucidation of the compounds' mechanisms of action. Objectives The main objective of this work was to develop a feasible and effective sample pretreatment method to measure the concentrations of resveratrol and polydatin in complex samples. Methodology A polymer sorbent, poly(2-mercaptobenzimidazole), was electrochemically prepared and utilized for selective extraction, while resveratrol and polydatin were used as target analytes. The sorbent was characterized by cyclic voltammetry, scanning electron microscopy and Fourier transform infrared spectroscopy. After extraction and elution, the analytes were analyzed by a Thermo U3000 HPLC system. Several affecting parameters, including the volume of elution solution, sample pH value, sample flow rate and sample volume, were evaluated and optimized. Results The proposed method showed good linearity with low limits of detection (from 0.5 to 0.8 ng center dot mL(-1)) and ideal accuracy with spiked recoveries from 81.30% to 99.16%. A good enrichment factor (more than 200-fold) together with good sensitivity was obtained with this method. Analysis of resveratrol and polydatin in Polygonum cuspidatum samples by this method is efficient. Conclusion The method developed in this work exhibits several significant merits, including easy operation and high extraction efficiency, indicating that electrochemically prepared polymer sorbent is useful for sample pretreatment and analysis of traditional Chinese medicine samples.
查看更多>>摘要：Introduction Astragali Radix has been used for over 2000 years in traditional Chinese medicine. Its secondary xylem "Jinjing" and secondary phloem "Yulan" are important for evaluating the quality of the Daodi medicinal material in China. However, its systematic characterisation has not been conducted. Objective This study aims to investigate the colour, chemical compounds, and antioxidant capacity of the secondary xylem and phloem of Astragali Radix on the basis of untargeted metabolomics, broadening the application scope of Astragali Radix in food and pharmaceutical industries. Methods The L*, a*, and b* of the secondary xylem and phloem were measured by colorimetry, and the chemical compounds were identified and quantified by ultra-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UPLC-Q-TOF-MS) and high-performance liquid chromatography-diode array detector-evaporative light scattering detection. 2,2-Diphenyl-1-picrylhydrazyl (DPPH) and 2-azino-bis-(3-ethylbenzothiazoline-6-sulphonic acid) (ABTS) assays were conducted to evaluate their antioxidant capacity. Results Thirty-one compounds were identified by UPLC-Q-TOF-MS. The secondary xylem exhibited high parameter b*, flavonoid content, and antioxidant capacity, while the secondary phloem was rich in astragalosides. The colour parameters of well-defined type A significantly varied from those of the other types. Well-defined type A also exhibited the highest antioxidant activity and flavonoid content, followed by middle type A-like, middle type B-like, and yellow shading type B. Conclusion The colour parameters, chemical compounds, and antioxidant capacity among the different transverse sections of secondary xylem and phloem varied. The yellow colour of secondary xylem was correlated to high flavonoid content and antioxidant activity, and well-defined type A of Astragali Radix had better quality than other types.
查看更多>>摘要：Introduction Tomentosin, the characteristic component of Inula viscosa (L.) is an important sesquiterpene lactone with anticarcinogenic effects. Methods of obtaining pure tomentosin are not sufficient for anticancer drug research. Objectives This study aims to develop a specific method to isolate tomentosin from I. viscosa with high yield. It also aims to investigate the inhibitory effects of tomentosin on human carbonic anhydrase I (hCAI), human carbonic anhydrase II (hCAII), acetylcholinesterase (AChE), butyrylcholinesterase (BChE), alpha-glucosidase, and alpha-amylase enzymes. Material and methods Tomentosin was purified by a specific column chromatography method. The content of tomentosin in dichloromethane, dichloromethane by Soxhlet method, ethanol and ethanol by Soxhlet method extracts of I. viscosa was determined by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Half maximal inhibitory concentration (IC50) and inhibition constant (K-i) values were calculated to determine in vitro enzyme inhibition effects. Results Tomentosin was isolated in high yield (0.64%). The IC50 and K-i values for tomentosin were calculated as 5.00 +/- 0.19 (r = 0.9688) and 4.62 +/- 0.10 mu M for hCAI, 5.40 +/- 0.26 (r = 0.9677) and 5.22 +/- 0.31 mu M for hCAII, 6.75 +/- 0.208 (r = 0.9891) and 3.75 +/- 0.27 mu M for AChE, 6.67 +/- 0.307 (r = 0.9820) and 0.51 +/- 0.11 mu M for BChE, 26.61 +/- 0.236 (r = 0.9815) and 2.61 +/- 0.71 mu M for alpha-glucosidase and 26.89 +/- 1.54 mu M (r = 0.9670) for alpha-amylase, respectively. Conclusion Tomentosin was isolated in high yield from the paste-like extract of I. viscosa compared to the positive controls, it was determined that tomentosin was weakly effective against hCAI, hCAII, AChE and BChE, but thoroughly effective against alpha-glucosidase and alpha-amylase. These results suggested that tomentosin has alpha-glucosidase and alpha-amylase inhibitor potential.
NSTL
Wiley