Identification, structure elucidation, and isomer differentiation of phenolic compounds of Chinese pepper cultivars by UPLC-ESI-Q-TOF-MS and their antioxidant activity.

A total of 43 compounds, including phenolic acids, flavonoids, lignans, and diterpene, were identified and characterized using UPLC-ESI-Q-TOF-MS coupled with UNIFI software. The identified flavonoids were mostly isomers of luteolin, apigenin, and quercetin, which were elucidated and distinguished for the first time in pepper cultivars. The use of multivariate data analytics for sample discrimination revealed that luteolin derivatives played the most important role in differentiating pepper cultivars. The content of phenolic acids and flavonoids in immature green peppers was generally higher than that of mature red peppers. The pepper extracts possessed significant antioxidant activities, and the antioxidant activities correlated well with phenolic contents and their molecular structure. In conclusion, the findings expand our understanding of the phytochemical components of the Chinese pepper genotype at two maturity stages. Moreover, a UPLC-ESI-Q-TOF-MS in negative ionization mode rapid methods for characterization and isomers differentiation was described.

Optimization of Ultrasound-Assisted Extraction of Verbascum sinaiticum Leaves: Maximal Phenolic Yield and Antioxidant Capacity.

Verbascum sinaiticum (Qetetina or yeahya Joro) is a medicinal plant with secondary metabolites such as phenolics, flavonoids, glycosides, saponins, and alkaloids. This study was designed to optimize the ultrasonic-assisted extraction (UAE) parameters to enhance the phenolic content and characterize the phenolic compounds using ultra-high-performance liquid chromatography, coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UHPLC-ESI-QTOF-MS/MS), and antioxidant activities in Verbascum sinaiticum extract. Extraction time, sample-to-solvent ratio, and extraction temperature were considered for UAE optimization. It was found that UAE generated the highest extraction yield (21.6%), total phenolic content (179.8 GAE mg/g), total flavonoid content (64.49 CE mg/g), DPPH (61.85 µg/mL), and ABTS (38.89 µg/mL) when compared to maceration extraction. Metabolite analysis in this study showed the detection of 17 phenolic compounds, confirming antioxidant capacities. The optimization parameters have significant effects on phenolic compounds. Scanning electron microscopy showed the presence of structural changes when UAE was used over the maceration method. The optimized UAE parameters for extraction temperature (41.43 °C), sample-to-solvent ratio (36.32 g/mL), and extraction time (33.22 min) for TPC were obtained. This study shows the potential application for UAE of Verbascum sinaiticum leaves in the development of pharmaceutical and nutraceutical products.

Light-Induced Antioxidant Phenolic Changes among the Sprouts of Lentil Cultivar.

Lentil is a leguminous crop with a high content of health-beneficial polyphenols. Lentil sprouts are popularly consumed in fresh vegetable markets, although their phytochemical qualities are not well understood. In this study, we investigated the accumulation of phenolics in lentil sprouts in response to photosynthetic and stress light qualities, including fluorescent light (FL), red LED (RL), blue LED (BL), ultraviolet A (UV-A), and ultraviolet B (UV-B). Three lentil cultivars, Lentil Green (LG), French Green (FG), and Lentil Red (LR), were used to evaluate sprouts grown under each light condition. The adequate light intensities for enhancing the antioxidant activity of lentil sprouts were found to be 11 W/m2 under photosynthetic lights (FL, RL, BL), and 1 W/m2 under stress lights (UV-A, UV-B). Subsequently, HPLC-ESI/Q-TOF MS analysis was conducted for the quantitative analysis of the individual phenolics that were accumulated in response to light quality. Four main phenolic compounds were identified: ferulic acid, tricetin, luteolin, and kaempferol. Notably, tricetin accumulation was significantly enhanced under BL across all three lentil cultivars examined. Furthermore, the study revealed that the other phenolic compounds were highly dependent on FL, BL, or UV-B exposure, exhibiting cultivar-specific variations. Additionally, the antioxidant activities of lentil extracts indicated that BL was most effective for LG and FG cultivars, whereas FL was most effective for enhancing antioxidant activity of LR cultivars as the sprouts grew.

Phenolic compounds profile of macerates of different edible parts of carob tree (Ceratonia siliqua L.) using UPLC-ESI-Q-TOF-MSE: Phytochemical screening and biological activities.

Locust bean pulp and gum extracts were prepared, and phytochemical tests based on color reactions and chromatographic analyzes were performed. A profile of seventy-six phenolic compounds was obtained by the ultra-high performance liquid chromatography with electrospray ionization and quadrupole time-of-flight mass spectrometry. The main groups of phenolic compounds identified in the both extracts of Ceratonia siliqua L., were flavonoids, tannins and phenolic acids. Moreover, carob pulp and gum extracts were tested for their antimicrobial activity using disk diffusion tests which showed sensitivity of the different strains to the analyzed extracts at a concentration of 100 mg/mL. Additionally, the antioxidant activity of Ceratonia siliqua L. extracts was assessed by the 2,2-diphenyl-1-picrylhydrazyl acid test, which confirmed stronger antioxidant properties in the case of the pulp extract. To sum up, carob pulp and gum extracts present promising alternatives to synthetic additives within the medicinal industry, serving as potential antioxidant agents and preservatives that combat bacterial contamination, thereby offering a more natural approach to enhancing product safety and efficacy.

Comprehensive metabolomic analysis of Mangifera indica leaves using UPLC-ESI-Q-TOF-MSE for cell differentiation: An in vitro and in vivo study.

The comprehensive metabolic profiling was performed in the leaf extracts of Mangifera indica and assessed for their significant therapeutic application in tissue engineering and regenerative medicine in both in vitro and in vivo studies. About 147 compounds were identified in the ethyl acetate and methanol extracts of M. indica using MS/MS fragmentation analysis and the selected compounds were quantified using LC-QqQ-MS analysis. The in vitro cytotoxic activity showed that the M. indica extracts enhance the proliferation of mouse myoblast cells in concentration-dependent manner. As well, the extracts of M. indica induce the myotube formation by generating oxidative stress in the C2C12 cells was confirmed. The western blot analysis clearly showed that the M. indica induce myogenic differentiation by upregulating the myogenic marker proteins such as PI3K, Akt, mTOR, MyoG, and MyoD. The in vivo studies showed that the extracts expedites the acute wound repair by formation of crust, wound closure and improves the blood perfusion towards the wound area. Together, the leaves of M. indica can be used as excellent therapeutic agent for tissue repair and wound healing applications.

Spectrochemical analysis of seasonal and sexual variation of antioxidants in Corema album (L.) D. Don leaf extracts.

Bioactive phytoconstituents have been increasingly investigated for their potential human health benefits. Corema album (L.) D. Don, an Ericaceae, reportedly has antioxidant, antimicrobial and anticancer properties. Aiming at enhancing its nutraceutical potential, we performed a spectrochemical analysis of hydroethanolic extracts from C. album leaves. We report on changes in the antioxidant activity of the extracts, as well as in the accumulation of key phytoconstituents (namely phenolic compounds), in female and male samples, throughout three harvesting seasons (February, July, and October). For each extract, the antioxidant activity was assessed by different spectrophotometric methods. Simultaneously, attenuated total reflectance Fourier transform mid-infrared spectroscopy (FTIR-ATR), and high-performance liquid chromatography - electrospray ionisation - quadrupole time-of-flight mass spectrometry (HPLC-ESI-Q-TOF-MS), were used to identify and monitor variations in the composition of phenolic compounds in the extracts. The main compounds identified were epicatechin, laricitrin-O-hexoside isomers, and myricetin-O-hexoside isomers. Significant differences were found in the composition and relative abundance of the compounds of interest, according to sex and season. Overall, a trend was observed whereby phenolic content and antioxidant activities were higher in males and increased between the earlier and the latest harvests. Based on these results, we may conclude that late summer or early autumn harvests are preferable when aiming at the highest yearly content of bioactive compounds. Additionally, it should be considered that extracts from male individuals typically display higher antioxidant activities. Ultimately, our understanding of C. album in the context of nutraceutical applications is benefited from the quantitative and qualitative portrait provided here, thus promoting its relevance as a source of bioactive compounds.

A comprehensive analysis of the chemical composition of Fraxinus mandshurica roots based on HPLC-DAD-MS, GC-MS and UPLC-ESI-Q-TOF-MS.

Fraxinus mandshurica is widely distributed around the world, which has significant economic value and pharmacological effects. However, its roots are often overlooked during processing and use. In this study, the preliminary identification of chemical components in F. mandshurica roots was carried out using ultra-performance liquid chromatography coupled with electrospray quadrupole time-of-flight mass spectrometry (UPLC-ESI-Q-TOF-MS), and a total of 37 characteristic components were identified, including 13 secoiridoids, 7 lignans, 6 coumarins, 4 flavonoids, 4 phenylethanols, 1 terpenoid and 2 other compounds. Meanwhile, to evaluate the 6 lignans content of F. mandshurica roots, the identification, quantitation analysis and methodological validation were performed by high-performance liquid chromatography with diode array detection mass spectrometry (HPLC-DAD-MS), which showed that the concentration range of standard compounds was 0.5-1000 µg/mL. The standard curve correlation coefficients (R2) were all greater than 0.9991, indicating that the linearity of the fitted curves was good. The highest lignan content in F. mandshurica roots was olivil (461.11 µg/g) and the lowest in buddlenol E (11.14 µg/g), and the total lignan content was 764.63 µg/g. The relative standard deviations (RSD, %) of both intra-day and inter-day precision were less than 1.95%. The RSD (%) of the reproducibility and stability experiments was less than 2.91%. The spiked recoveries of the samples were in the range of 98.29-102.62%, and the RSD (%) was in the range of 0.43-1.73, indicating that the method has high accuracy. In addition, a total of 20 volatile components in F. mandshurica roots were identified and quantified by gas chromatography-mass spectrometer (GC-MS) in this study, which laid a solid foundation for the comprehensive development and utilization of F. mandshurica resources.

Development of an online UPLC-PDA-ESI-Q-TOF-MS-LOX-FLD system for rapid screening of anti-inflammatory compounds in Polygala tenuifolia Willd.

In this study, the first ultra-high performance liquid chromatography-photo-diode array-electrospray ionization-quadrupole-time-of-flight-mass spectrometry-lipoxygenase-fluorescence detector (UPLC-PDA-ESI-Q-TOF-MS-LOX-FLD) online system was developed for the identification and evaluation of anti-inflammatory active ingredients in Polygala tenuifolia Willd. Using this system, the UPLC fingerprints, mass fragments and LOX-binding peak profiles in the samples were rapidly and simultaneously obtained. A total of 101 compounds were isolated and identified and 38 compounds (11 oligosaccharide esters, nine xanthones, 17 saponins, and one glycosyloxyflavone) showed strong LOX-binding activity. Six compounds were selected to study their LOX-binding ability, and the results indicated that the content of the six compounds had a good linear relationship with the LOX-binding ability, and it was found that the substitution position, the type of substituent and the number of glycosyl groups all had a certain influence on the LOX-binding ability of the compounds. The LOX-binding activities of 10 compounds were verified by the surface plasmon resonance (SPR) technique and the activity results were consistent with the online system. After validation, we identified 7 active compounds that combined with LOX to exert anti-inflammatory effects for the first time. All the results fully demonstrate the efficiency, stability and reliability of the online system and this work provides an exemplary and useful method for the rapid screening of potential anti-inflammatory active compounds in P. tenuifolia and other traditional Chinese medicines. At the same time, it provides a new direction for screening small molecule inhibitors of enzymes like LOX.

Bupleurum scorzonerifolium: Systematic research through pharmacodynamics and serum pharmacochemistry on screening antidepressant Q-markers for quality control.

Bupleurum scorzonerifolium (BS) is one of the sources of Bupleuri Radix, which was first recorded in Shennong's classic of materia medica. It has a medicinal history of 2000 years and is now widely used for the treatment of depression clinically. However, the material basis of antidepressant effects is unclear, and the quality evaluation method is lacking. The paper aims to investigate the antidepressant quality markers (Q-markers) of BS by electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UPLC-ESI-Q-TOF-MS). Firstly, the rat depression model was established by using chronic unpredictable mild stress (CUMS) combined with the solitary confinement method to evaluate the pharmacodynamics of BS. After verification of the antidepressant effect of BS, UPLC-ESI-Q-TOF-MS was used to analyze BS and the blood components of BS. A total of 34 components were identified in BS, in which 8 components, including saikosaponin a (SSa), saikosaponin c (SSc), saikosaponin d (SSd), saikosaponin b1 (SSb1), saikosaponin b2 (SSb2), glycyrrhetinic acid, nootkatone and valerenic acid, were detected in serum. SSa, SSc, SSd, SSb1 and SSb2 were found as metabolites, and glycyrrhetinic acid, nootkatone and valerenic Acid were identified as the prototypes in the blood. The depression model of zebrafish was established with reserpine to verify the antidepressant effect of the potential eight active components. The results showed that all these components could markedly improve the depressive behavior of zebrafish, increase the content of 5-HT and reduce the cortisol content. Finally, according to the principles of effectiveness, accessibility and measurability for Q-markers, SSa, SSc, and SSd were confirmed as Q-markers of BS, and the contents of 3 Q-markers in 10 batches of BS from different origins were determined to be 0.0728-1.465%. In addition, the total contents of 3 Q-markers in BS produced in Lindian, Heilongjiang Province, were higher than those in other origins. This paper provided a reliable method for the quality evaluation of BS for depression treatment.

Metabolomic Study of Urine from Workers Exposed to Low Concentrations of Benzene by UHPLC-ESI-QToF-MS Reveals Potential Biomarkers Associated with Oxidative Stress and Genotoxicity.

Benzene is a human carcinogen whose exposure to concentrations below 1 ppm (3.19 mg·m-3) is associated with myelotoxic effects. The determination of biomarkers such as trans-trans muconic acid (AttM) and S-phenylmercapturic acid (SPMA) show exposure without reflecting the toxic effects of benzene. For this reason, in this study, the urinary metabolome of individuals exposed to low concentrations of benzene was investigated, with the aim of understanding the biological response to exposure to this xenobiotic and identifying metabolites correlated with the toxic effects induced by it. Ultra-efficient liquid chromatography coupled to a quadrupole-time-of-flight mass spectrometer (UHPLC-ESI-Q-ToF-MS) was used to identify metabolites in the urine of environmentally (n = 28) and occupationally exposed (n = 32) to benzene (mean of 22.1 µg·m-3 and 31.8 µg·m-3, respectively). Non-targeted metabolomics analysis by PLS-DA revealed nine urinary metabolites discriminating between groups and statistically correlated with oxidative damage (MDA, thiol) and genetic material (chromosomal aberrations) induced by the hydrocarbon. The analysis of metabolic pathways revealed important alterations in lipid metabolism. These results point to the involvement of alterations in lipid metabolism in the mechanisms of cytotoxic and genotoxic action of benzene. Furthermore, this study proves the potential of metabolomics to provide relevant information to understand the biological response to exposure to xenobiotics and identify early effect biomarkers.

Suppression of Pepper mild mottle virus (PMMoV) by Modified Whey Proteins.

Modified whey proteins with quercetin (WPI-QU) and onion extract (WPI-OE), as a control approach, could be applicable because it is available, safe and cheap. The modified whey protein isolate (WPI) with quercetin dihydrate and onion extract powder rich with quercetin were evaluated for induction of systemic resistance against Pepper mild mottle virus (PMMoV) in pepper plants. Data of mass spectrometry illustrated that one or more of Qu isomers covalently attached to WPI. Unmodified whey protein (UWPI), WPI-QU and WPI-OE significantly decreased PMMoV concentration and severity at two weeks after inoculation. Plant height, number of leaves, and shoot fresh and dry weights were substantially increased in WPI-QU- and WPI-OE-treated pepper plants compared to the control. Total antioxidant status (TAS) and vitamin C contents were highly increased in WPI-OE-treated plants compared with other treatments. The expression levels of defense related genes (PR4, PR9, TIN1 and PIN2) were enormously elevated in WPI-OE and WPI-QU treatments using qRT-PCR. In conclusion, the results give novel insights to possible applications of the WPI-quercetin bioconjugates in designing a wide range of functional products. Moreover, this study is the first to establish the effective control of PMMoV by modified whey proteins.

Chemical profiling of marine seaweed Halimeda gracilis using UPLC-ESI-Q-TOF-MSE and evaluation of anticancer activity targeting PI3K/AKT and intrinsic apoptosis signaling pathway.

Marine seaweeds are predominant for nutraceuticals and have been food source since ancient times and are currently being used in Chinese medicines and Japanese traditional medicines. In the present study, the chemical profile analysis of Halimeda gracilis was performed using UPLC-ESI-Q-TOF-MSE analysis and assessed for its anticancer activity. A cursory investigation of the total ion chromatograms of the both methanol (MHG) and ethyl acetate (EAHG) of H. gracilis extracts reveals that both extracts have different kind of metabolites including phenols and its derivatives, diterpenes, cinnamic acids derivatives etc. The in vitro anticancer activity of EAHG and MHG exhibiting significant activity and induced apoptosis against skin cancer cells by generating excessive ROS, damaging the mitochondrial membrane and nuclear components. Further, the western blot analysis showed that the EAHG and MHG downregulates the oncoproteins PI3K, AKT, p-AKT, and BcL2 and upregulates the apoptotic proteins Bax, Cyto C, p21, p53, Caspase 9 and Caspase 3. To best of our knowledge, this is the first report which implies the UPLC-ESI-Q-TOF-MSE based chemical profiling of H. gracilis and can be used for the treatment of cancer.

Apigenin glycosides from green pepper enhance longevity and stress resistance in Caenorhabditis elegans.

Peppers are a rich source of bioactive compounds with several health benefits. However, most of the knowledge about these benefits has been obtained through in vitro studies, and less is known about their in vivo health-promoting and stress resistance effects. Therefore, we hypothesized that the intake of apigenin glycosides (XAp-G) from Xiaomila green pepper (Capsicum frutescens) could protect against stress factors and promote longevity of Caenorhabditis elegans. Synchronized worms were treated with XAp-G and the lifespan and stress resistance were examined. XAp-G treatment strongly enhanced the average lifespan of worms by 23.9% compared with control by reducing the reactive oxygen species (ROS) level. Ultrahigh performance liquid chromatography-electrospray ionization-quadrupole time-of-flight mass spectometry analysis showed that Xiaomila pepper (polyamide fraction) contained significant amount of flavone glycosides with m/z 563.14 (apigenin glycosides). Green fluorescent protein fluorescence and real-time polymerase chain reaction analyses showed that XAp-G-treatment could regulate the expression of anti-aging related genes, including daf-2, daf-16, sod-3, hsp-16.2, skn-1, gst-4, gcs-1, jnk-1, and sir-2.1 in C elegans, thereby promoting the translocation of DAF-16 and SKN-1 into the nucleus. However, it could not extend the lifespan of daf-16, skn-1, and sir-2.1 knocked-down mutants. XAp-G treatment significantly reduced ROS under normal and stress conditions (juglone, hydrogen peroxide), and thereby promotes longevity of C elegans via the insulin/insulin-like growth factor-1 signaling pathway.

Capsaicinoid-Glucosides of Fresh Hot Pepper Promotes Stress Resistance and Longevity in Caenorhabditis elegans.

In this study, capsaicin-glucoside and dihydro-capsaicin-glucoside derived from fresh hot-red pepper were isolated and identified using UPLC-ESI-Q-TOF-MS/PDA. Synchronized worms were treated with capsaicinoid-glucosides (CG), and then lifespan and stress resistance were examined. The 50 µg/ml concentration of CG-intake could effectively protect the Caenorhabditis elegans (C. elegans) against stresses factors including oxidation and heat as well as reactive oxygen species (ROS), thereby enhancing the survival of CG-treated worms under stress. Enhancing stress resistance in CG-treated worms could be due to the increased expressions of stress-related genes in C. elegans such as daf-16, skn-1 and their downstream target genes (sod-3, hsp-16.2, gst-4 and gcs-1). Lifespan study of different C. elegans strains and RT-PCR showed that the CG-mediated lifespan extension was dependent on DAF-16/FOXO and SKN-1/Nrf2 transcription factors. The study is a step forward in exploring the stress resistance and anti-aging properties of this beneficial extract. Thus, this study will be useful in formulating remedies for stresses factors and age associated disorders.

Identification of potential serum metabolic biomarkers for patient with keratoconus using untargeted metabolomics approach.

This study aimed to investigate the metabolite differences between patients with keratoconus and control subjects and identify potential serum biomarkers for keratoconus using a non-targeted metabolomics approach. Venous blood samples were obtained from patients with keratoconus (n = 20) as well as from age-, gender- and race-matched control subjects (n = 20). Metabolites extracted from serum were separated and analyzed by liquid chromatography/quadrupole time-of-flight mass spectrometer. Processing of raw data and analysis of the data files was performed using Agilent Mass Hunter Qualitative software. The identified metabolites were subjected to a principal component and hierarchical cluster analysis. Appropriate statistical tests were used to analyze the metabolomic profiling data. Together, the analysis revealed that the dehydroepiandrosterone sulfate from the steroidal hormone synthesis pathway was significantly upregulated in patients with keratoconus (p < 0.05). Also, a combination of eicosanoids from the arachidonic acid pathway, mainly prostaglandin F2α, prostaglandin A2, 16,16-dimethyl prostaglandin E2, and 5-hydroxyeicosatetraenoic acid were collectively up-regulated as a group in keratoconus patients (p < 0.05). On the other hand, glycerophospholipid PS(17:2(9Z,12Z)/20:4(5Z,8Z,11Z,14Z)) was found to be significantly upregulated in the metabolomics profiles of control subjects (p < 0.05). The differently regulated metabolites provide insights into the pathophysiology of keratoconus and could potentially be used as biomarkers for keratoconus to aid in screening for individuals at risk hence, enabling early diagnosis and timely monitoring of disease.

Evaluation of lipid profiles in three species of ascidians using UPLC-ESI-Q-TOF-MS-based lipidomic study.

Ascidians are excellent, yet underused, marine sources of unique bioactive compounds of high nutritive content. However, reports regarding the lipid composition of ascidians are rare. In this study, using ultra-high-performance liquid chromatography-electrospray ionization-quadrupole time-of-flight mass spectrometry, we aimed to characterize the lipid profile of the tunics and inner body tissues of three species of ascidians, including Ciona intestinalis, Halocynthia roretzi, and Styela clava. We identified over 245 molecular species from 13 major lipid subclasses; glycerophospholipids (GP) and glycerolipids were the dominant lipid components in these three ascidian species (accounted for 66.30-90.60% of total lipids). Importantly, GP enriched in polyunsaturated fatty acids mainly existed in the inner body tissues of ascidians, which accounted for 18.17-32.47% of total lipids. Considering the high level of GP, we proposed that ascidians can be potentially used as health-promoting food for humans.

Systematically identifying the anti-inflammatory constituents of Cimicifuga dahurica by UPLC-Q/TOF-MS combined with network pharmacology analysis.

Cimicifuga dahurica (Turcz.) Maxim, which is also regarded as the main origin of "Shengma" in the Chinese Pharmacopoeia, has been used as a cooling and detoxification agent for thousands of years. Our previous phytochemical investigations of C. dahurica extracts (CDEs) led to the isolation of a series of 9,19-cycloalkane triterpenoids and phenolic acids showing a potential anti-inflammatory activity. However, the chemical profiling of CDEs and the material basis of its anti-inflammatory effect in vivo has not been clarified. In the present study, the CDE chemical profile and prototype components in rat plasma were identified via ultra-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry. As a result, a total of 106 components were identified or tentatively characterized in CDEs, including 54 triterpenoids, 35 phenolic acids, eight amides and nine other type constituents (39 compounds were confirmed with the reference standards). In addition, 20 prototype components (15 triterpenoids and five phenolic acids) were identified in rat plasma, which potentially related to the anti-inflammatory effects of CDEs. Moreover, the anti-inflammatory activities of the main prototype components were further evaluated by their inhibitory effects on the production of NO, as well as the expressions of iNOS and COX-2 in lipopolysaccharide-stimulated RAW264.7 cells, which indicated that 9,19-cycloalkane triterpenoids may play an anti-inflammatory role by down-regulating the expression of iNOS.

Studies on effect of Tongfengxiaofang in HUM model mice using a UPLC-ESI-Q-TOF/MS metabolomic approach.

Hyperuricemia (HUM) is a major risk factor for the development of gout. The traditional Chinese medicine (TCM) complex prescription Tongfengxiaofang (TFXF) is composed of a variety of TCMs. To study the therapeutic effect of TFXF on HUM mice and the mechanisms by which it exerts a therapeutic effect, the biochemical indices were measured and qPCR technique was used. In addition, plasma metabolomics analysis was carried out based on UPLC-Q-TOF/MS to evaluate the characteristics of the metabolic spectrum changes. TFXF significantly downregulated the contents of uric acid, urea nitrogen and creatinine in serum and the concentration of xanthine oxidase in liver of HUM mice. In addition, TFXF significantly inhibited the overexpression of uric acid transporter 1 and glucose transporter 9 and upregulated the expression of organic anion transporter 1 in the kidney. A total of 152 metabolites were identified and 11 key biomarkers were further selected from these pathways to understand the mechanism of TFXF on the arginine biosynthesis, galactose metabolism, pyrimidine metabolism, glycerophospholipid metabolism, tryptophan metabolism and the citrate cycle (TCA cycle). The results of this confirmed the effect of TFXF on HUM and revealed the metabolic activity mechanism.

Characterization of lipid profiling in three parts (muscle, head and viscera) of tilapia (Oreochromis niloticus) using lipidomics with UPLC-ESI-Q-TOF-MS.

A lipidomic evaluation was performed on the tilapia muscle, head and viscera, including studying the composition, distribution and stereospecific characteristics of fatty acids and lipid species. The head and viscera lipids were significantly richer than the muscle lipids. Triacylglycerols were the predominant fraction (over 80% of total lipid in the muscle and head). Additionally, polyunsaturated fatty acids had higher percentages in phospholipids (30.35-52.05% of total fatty acids) than in triacylglycerols (18.11-25.15%). The C52:2 and C52:3 were the most abundant triacylglycerols, which indicates the potential application in infant food. Moreover, 622, 530 and 513 lipids were identified using ultraperformance liquid chromatography-quadrupole time-of-flight-mass spectrometry in the muscle, head and viscera, respectively. The three tilapia parts were distinguished using multivariate analysis. Five fatty acids and 33 lipid species were considered as the potential biomarkers. This comprehensive analysis will help to evaluate the lipid nutritional values and facilitate exploitation in tilapia consumption and processing.

MS diagnostic model and rapid distinguishing of bioactive limonoids in fruits of Melia toosendan using solid-phase extraction coupled with LC-MS/MS.

INTRODUCTION: Melia toosendan Sieb. et Zucc. has been used as a Chinese folk medicine for roundworm treatment since ancient times. Many diverse limonoids have been isolated from Meliaceae plants, but it remains difficult to isolate and identify other limonoids because of their small natural concentrations. OBJECTIVE: This study was performed to overcome the difficulties associated with fast and accurate identification of limonoids and establish a reliable and sensitive method for the analysis of minor limonoids in M. toosendan fruits. METHODS: An efficient strategy for enrichment, detection, and identification of minor limonoids from M. toosendan fruits using solid-phase extraction with high-performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry (SPE-HPLC-Q-TOF-MS/MS) was developed herein. RESULTS: Characteristic fragmentations and fragmentation ions containing trichilin-, nimbin-, and vilasinin-class limonoid skeletons were initially studied, and characteristic diagnostic ions involved retro Diels-Alder (RDA) reactions or homolytic cleavages, which were used to identify minor limonoids. In total, 13 limonoids, including four new ones, were identified. CONCLUSION: This is the first report on the analysis of M. toosendan fruits to identify limonoids. This novel analysis method may stimulate further research regarding the identification of limonoids in other plant species.