Ultra-performance Liquid Chromatography-electrospray Ionization Research Articles

Differential Extraction and Preliminary Identification of Polyphenols from Ugni candollei (White Murta) Berries

Ugni candollei, commonly known as white murta, is a native Chilean berry with a polyphenol composition that has been underexplored. This study aimed to establish a comprehensive profile of white murta polyphenols using ultra-performance liquid chromatography electrospray ionization Orbitrap mass spectrometry (UPLC-ESI-ORBITRAP MS). Additionally, it compared the efficacy of conventional extraction methods with emerging techniques such as deep eutectic solvent (DES) extraction and hot pressurized water extraction (HPWE). The analysis tentatively identified 107 phenolic compounds (84 of them reported for the first time for this cultivar), including 25 phenolic acids, 37 anthocyanins, and 45 flavonoids. Among the prominent and previously unreported polyphenols are ellagic acid acetyl-xyloside, 3-p-coumaroylquinic acid, cyanidin 3-O-(6′-caffeoyl-glucoside, and phloretin 2′-O-xylosyl-glucoside. The study found HPWE to be a promising alternative to traditional extraction of hydroxybenzoic acids, while DES extraction was less effective across all categories. The findings reveal that white murta possesses diverse phenolic compounds, potentially linked to various biological activities.

Untargeted Metabolomic Profiling of Fructus Chebulae and Fructus Terminaliae Billericae

This study aims to identify the differences in metabolites between Fructus Chebulae (FC) and Fructus Terminaliae Billericae (FTB). Untargeted metabolomics was used to analyze differentially expressed metabolites (DEMs) with ultra-performance liquid chromatography–electrospray ionization–tandem mass spectrometry (UPLC-ESI-MS/MS). A grand total of 558 metabolites were detected, with 155 in positive ion mode and 403 in negative ion mode. Further differential analysis yielded 110 and 87 significantly different metabolites, which were mainly polyphenols, flavonoids, terpenoids, and alkaloids. Analysis of KEGG data showed that differentially expressed metabolites (DEMs) in both positive and negative ion modes were found to be enriched in 5 and 18 metabolic pathways, respectively, with metabolic pathways being the most enriched among them. In sum, this study reveals the differential metabolic profiles of FC and FTB and provides support for their further applications in traditional Chinese medicine.

Phytochemical profile and anti-inflammatory activity of the hull of γ-irradiated wheat mutant lines (Triticum aestivum L.).

Wheat (Triticum aestivum Linn.; Poaceae) is the second most cultivated food crop among all global cereal crop production. The high carbohydrate content of its grains provides energy, multiple nutrients, and dietary fiber. After threshing, a substantial amount of wheat hull is produced, which serves as the non-food component of wheat. For the valorization of these by-products as a new resource from which functional components can be extracted, the hull from the seeds of cultivated wheat mutant lines bred after γ-irradiation were collected. Untargeted metabolite analysis of the hull of the original cultivar (a crossbreeding cultivar., Woori-mil × D-7) and its 983 mutant lines were conducted using ultra-performance liquid chromatography-electrospray ionization quadrupole time-of-flight mass spectrometry technique. A total of 55 molecules were tentatively identified, including 21 compounds found in the Triticum species for the first time and 13 compounds not previously described. Among them, seven flavonolignans with a diastereomeric structure, isolated as a single compound from the hull of T. aestivum in our previous study, were used as the standards in the metabolite analysis. The differences in their collision cross-section values were shown to contribute to the clear distinction between tricine-lignan stereoisomers. To select functionally active agents with anti-inflammatory activity among the identified compounds, the wheat hull samples were evaluated for their inhibitory effect on nitric oxide production in lipopolysaccharide-stimulated RAW 264.7 cells. As a result of multivariate analysis based on the results of chemical and biological profiles of the wheat hull samples, 10 metabolites were identified as key markers, contributing to the distinction between active and inactive mutant lines. Considering that one of the four key markers attributed to anti-inflammatory activity has been identified to be a flavonolignan, the wheat hull could be a valuable source of diverse tricin-lignan type compounds and used as a natural health-promoting product in food supplements.

Parallel artificial liquid membrane extraction coupled with UPLC-ESI-MS/MS method for high-throughput quantitation of repaglinide in diabetic patients

A high-throughput therapeutic monitoring method was developed for repaglinide (RPG) in diabetic patients, combining parallel artificial liquid membrane extraction (PALME) with ultraperformance liquid chromatography electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS). PALME was performed using a 96-well donor plate comprising a donor solution containing a plasma sample, 50 mM phosphate buffer (pH = 8.0), and cetirizine (CTZ) as internal standard. A polypropylene (PP) porous membrane served as a selective support for the liquid membrane (SLM), preventing nonspecific binding produced by other membranes. The extraction was accomplished across SLM made of PP membrane with dodecyl acetate and 1 % trioctylamine (w/w), and the acceptor solution comprised DMSO and 200 mM formic acid (50:50, v/v). The simple workflow for PALME provided analyte enrichment, highly efficient sample cleanup, high throughput analysis, and excellent reproducibility. Method validation met FDA criteria, with a linear plasma calibration range (0.1–100 ng mL−1, r = 0.9995) and a lower limit of quantitation (LLOQ) of 0.1 ng mL−1. Recovery results at 98.9 % affirmed method reliability. The ability to analyze 198 samples per hour, coupled with a reduced amount of solvents, underscores the method's high throughput and eco-friendly profile. The PALME-UPLC-ESI-MS/MS method was successfully applied to therapeutic drug monitoring of RPG in diabetic patients following 2 mg RPG tablet administration, establishing its effectiveness.

Functional Characterization of AP2/ERF Transcription Factors during Flower Development and Anthocyanin Biosynthesis Related Candidate Genes in Lycoris.

The APETALA2/ethylene-responsive transcription factor (AP2/ERF) family has been extensively investigated because of its significant involvement in plant development, growth, fruit ripening, metabolism, and plant stress responses. To date, there has been little investigation into how the AP2/ERF genes influence flower formation and anthocyanin biosynthesis in Lycoris. Herein, 80 putative LrAP2/ERF transcription factors (TFs) with complete open reading frames (ORFs) were retrieved from the Lycoris transcriptome sequence data, which could be divided into five subfamilies dependent on their complete protein sequences. Furthermore, our findings demonstrated that genes belonging to the same subfamily had structural similarities and conserved motifs. LrAP2/ERF genes were analyzed for playing an important role in plant growth, water deprivation, and flower formation by means of gene ontology (GO) enrichment analysis. The expression pattern of the LrAP2/ERF genes differed across tissues and might be important for Lycoris growth and flower development. In response to methyl jasmonate (MeJA) exposure and drought stress, the expression of each LrAP2/ERF gene varied across tissues and time. Moreover, a total of 20 anthocyanin components were characterized using ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) analysis, and pelargonidin-3-O-glucoside-5-O-arabinoside was identified as the major anthocyanin aglycone responsible for the coloration of the red petals in Lycoris. In addition, we mapped the relationships between genes and metabolites and found that LrAP2/ERF16 is strongly linked to pelargonidin accumulation in Lycoris petals. These findings provide the basic conceptual groundwork for future research into the molecular underpinnings and regulation mechanisms of AP2/ERF TFs in anthocyanin accumulation and Lycoris floral development.

Mineral composition, principal polyphenolic components, and evaluation of the anti-inflammatory, analgesic, and antioxidant properties of Cytisus villosus Pourr leaf extracts

Abstract Cytisus villosus Pourr. (C. villosus) is a medicinal plant belonging to the Fabaceae family, which grows in the Mediterranean area. It is used in traditional medicine against diseases related to inflammation. The objective of the present study was to identify the mineral and polyphenolic composition as well as to evaluate some biological properties including antioxidant, anti-inflammatory, and analgesic activities of C. villosus leaf aqueous extract. The chemical constituents were identified and quantified using ultra performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) methods. The antioxidant properties of C. villosus leaves were tested using reducing power (RP), 2,2-azino-bis-3-ethylbenzothiazoline-6-sulfonic acid (ABTS), and 2,2′-diphenyl-1-picrylhydrazyl (DPPH) assays. The anti-inflammatory potency was evaluated in vitro and in vivo using the albumin denaturation test and the carrageenan test, respectively. Furthermore, the analgesic effect was performed in vivo using tail flick, acetic acid-induced contortion, and plantar tests. Mineralogical analysis revealed that potassium and calcium were the most abundant minerals. The analysis and quantification of the phytochemical composition using UPLC-ESI-MS/MS showed that quinic acid (57.478 ± 1.72 mg/kg) was the major compound of the aqueous extract, followed by salicylic acid (17.38 ± 0.2 mg/kg), isoquercetin (16.895 ± 1.01 mg/kg), and gallic acid (15.914 ± 1.51 mg/kg). The extracts showed potent antioxidant activity for all tests used. The highest antioxidant activity was recorded for the DPPH, ABTS and RP methods, with an IC50 of 3.94 ± 0.09, 2.88 ± 0.07, and 1.94 ± 0.10 μg/mL, respectively. Additionally, using the most frequent analgesic assays, the aqueous extract at a dose of 500 mg/kg exhibited a potent analgesic activity. Notably, an interesting inhibition of albumin denaturation was recorded with an IC50 of 383.94 μg/mL, corroborating the in vivo test. Overall, the results presented here may represent a scientific basis for the traditional use of C. villosus in the treatment of inflammation-related diseases.

Liver lipidomics analysis reveals the anti-obesity and lipid-lowering effects of gypnosides from heat-processed Gynostemma pentaphyllum in high-fat diet fed mice

BackgroundIn traditional Chinese medicine, Gynostemma pentaphyllum (G. pentaphyllum) is widely used to treat conditions associated with hyperlipidemia, and its therapeutic potential has been demonstrated in numerous studies. However, the mechanism of lipid metabolism in hyperlipidemic by G. pentaphyllum, especially heat-processed G. pentaphyllum is not yet clear. PurposeThe aim of this study was to investigate the therapeutic mechanism of gypenosides from heat-processed G. pentaphyllum (HGyp) in hyperlipidemic mice by means of a lipidomics. MethodsThe content of the major components of HGyp was determined by ultra-performance liquid chromatography-electrospray ionization ion trap mass spectrometry (UPLC-ESI-MS). An animal model of hyperlipidaemia was constructed using C57BL/6J mice fed with high-fat diet. HGyp was also administered at doses of 50, 100 and 200 mg/kg, all for 12 weeks. Serum parameters were measured, histological sections were prepared and liver lipidome analysis using UPLC-MS coupled with multivariate statistical analysis. Quantitative real-time polymerase chain reaction (qRT-PCR) and western blotting were used to analyze the genes and proteins associated with lipid lowering in HGyp. ResultsHGyp reduced body weight, serum total cholesterol (TC), triglyceride (TG) and low-density lipoprotein (LDL) and hepatic lipid accumulation in hyperlipidemic obese mice. To explore specific changes in lipid metabolism in relation to HGyp administration, lipid analysis of the liver was performed. Orthogonal partial least squares discriminant analysis (OPLS-DA) score plots showed that HGyp altered lipid metabolism in HFD mice. In particular, fatty acids (FA), triglycerides (DG), TG and ceramides (CER) were significantly altered. Eleven lipids were identified as potential lipid biomarkers, namely TG (18:2/20:5/18:2), TG (18:2/18:3/20:4), DG (18:3/20:0/0:0), Cer (d18:1/19:0), Cer (d16:1/23:0), Ceramide (d18:1/9Z-18:1), PS (19:0/18:3), PS (20:2/0:0), LysoPC (22:5), LysoPE (0:0/18:0), PE (24:0/16:1). Western blot and qRT-PCR analysis showed that these metabolic improvements played a role by down-regulating genes and proteins related to fat production (SREBP1, ACC1, SCD1), up-regulating genes and proteins related to lipid oxidation (CPTA1, PPARα) and lipid transport decomposition in the bile acid pathway (LXRα, PPARγ, FXR, BSEP). ConclusionThe lipid-lowering effect of gypenosides from heat-processed G. pentaphyllum is regulate lipid homeostasis and metabolism.

Assessment of lipid composition and eicosapentaenoic acid/docosahexaenoic acid bioavailability in fish oil obtained through different enrichment methods.

In this study, we analyzed the eicosapentaenoic acid/docosahexaenoic acid (EPA/DHA) lipid composition of fish oil obtained through enzymatic treatment, fractional distillation and silica gel column purification, and further assessed EPA/DHA bioavailability. Lipid subclass composition information was obtained through ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS), and bioavailability tests were performed using the Caco-2 cell monolayer model. Results showed that enzymatic treatment improved the incorporation of EPA/DHA as diacylglycerol (DG) while silica gel column chromatography enriched the content of EPA/DHA as phosphatidylglycerol (PG) (12.58%) and phosphatidylethanolamine (PE) (4.99%). Furthermore, increasing the purity of EPA/DHA could improve its bioavailability and after 24 incubation, binding forms of triglyceride (TG) was superior to ethyl ester (EE) (p < 0.05) at the same purity level. Those findings are helpful to provide research basis for exploring the bioactivity of fish oil.

Anti-Inflammatory, Antioxidant Activities, and Phytochemical Characterization of Edible Plants Exerting Synergistic Effects in Human Gastric Epithelial Cells

Dietary bioactive compounds from natural sources (e.g., herbal medicines, foods) are known to potentially suppress acute or chronic inflammation and promote the effectiveness of treatment to reduce the harmful effects of gastritis alone or in combination. In this regard, we have characterized four Cameroonian spice extracts, namely Aframomum citratum, Dichrostachys glomerata, Tetrapleura tetraptera, and Xylopia parviflora through reverse phase-high-performance liquid chromatography (RP-HPLC), ultra-performance liquid chromatography-electrospray ionization high-resolution mass spectrometry (UPLC-ESI-HRMS/MS), and Fourier transform infrared spectroscopic (FTIR) analyses and investigated their antioxidant and synergistic anti-inflammatory activities in human gastric adenocarcinoma (AGS) and gastric epithelial (GES-1) cells. The extracts showed a high amount of total phenolic (TPC: 150-290 mg gallic acid equivalents (GAE)/g of extract) and flavonoid content (TFC: 35-115 mg catechin equivalents (CE)/g of extract) with antioxidant properties in a cell-free system (1,1-Diphenyl-2-picryl-hydrazyl (DPPH) half maximal inhibitory concentration (IC50s) ≤ 45 µg/mL; 2,2'-azinobis-(3-ethylbenzothiazoline-6-sulfonic acid) (ABTS) half maximal inhibitory concentration (IC50s) ≤ 29 µg/mL. The extracts in combination (MIX) exert a synergistic beneficial effect (combination index (CIs) < 1 and dose reduction index (DRIs) > 1) on inflammatory markers (interleukin (IL)-8 and -6 release, and nuclear factor kappa B (NF-κB) driven transcription) in human gastric epithelial cells, which may result from the presence of phenolic compounds (phenolic acids, flavonoids) or other compounds (protein, lipid, aromatic, and polysaccharide compounds) tentatively identified in the extracts. The general findings of the present study provide supporting evidence on the chemical composition of four Cameroonian dietary plants and their significant synergistic inhibitory activities on inflammatory markers of gastric epithelial cells.

Aqueous Extracts of Four Medicinal Plants and Their Allelopathic Effects on Germination and Seedlings: Their Morphometric Characteristics of Three Horticultural Plant Species

Allelopathy is a biological phenomenon of synthesizing and excreting compounds that can affect the growth of various organisms, i.e., plant species. The aim of this work was to investigate the possible allelopathic influence of aqueous extracts, obtained from plant species chia (Salvia hispanica L.), black cumin (Nigella sativa L.), wormwood (Artemisia absinthium L.), and nettle (Urtica dioica L.), on the seed germination growth and morphometric characteristics of pepper (Capsicum annuum L.), spinach (Spinacia oleracea L.) and lettuce (Lactuca sativa L.) seedlings in laboratory conditions. Pepper, spinach, and lettuce seedlings were treated with aqueous extracts of chia, nettle, wormwood, and black cumin of different concentrations (2.5, 5 and 10%, respectively). The aqueous extracts were prepared according to the method developed by Norsworthy and the qualitative and quantitative analysis of phenolic compounds in aqueous extracts were performed using ultra-performance liquid chromatography electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS). Phytochemical composition of chia aqueous extracts showed the highest content (above the 1 mg L−1) of epicatechin, quinic acid, caffeic acid, esculetin and cinnamic acid in the comparison with others from the total of 19 detected chemical compounds. In aqueous extracts of black cumin, there were six compounds detected in content above 1 mg L−1, i.e., epicatechin, quinic acid, caffeic acid, esculetin, cinnamic acid, and kaempferol. The same compounds were the most abundant in wormwood extracts, along with gallic acid. Epicatechin and esculetin were only two compounds detected in aqueous extract of nettle in concentration higher than 1 mg L−1. According to the results of this study, only the treatment of spinach seeds with chia aqueous extract in concentration of 2.5% before germination stimulates the germination of spinach seeds, and wormwood herbs and chia extracts in concentrations of 2.5 and 5% stimulate the germination of lettuce seeds and the growth of hypocotyl and radicle length of developed seedlings. The treatment of pepper and lettuce seeds with aqueous extract of nettle in concentration of 10% completely inhibited seed germination.

Metabolites Profiling and In Vitro Biological Characterization of Different Fractions of Cliona sp. Marine Sponge from the Red Sea Egypt.

Red Sea marine sponges are an important source of biologically active natural products. Therefore, the present study aimed to investigate, for the first time, the components of n-hexane, dichloromethane, and ethyl acetate fractions of Cliona sp. marine sponge collected from the Red Sea, Egypt using UPLC-ESI-MS/MS (Ultra-performance liquid chromatography electrospray ionization tandem mass spectrometry) analysis. The analysis revealed the tentative identification of 23, 16, and 24 compounds from the n-hexane, dichloromethane, and ethyl acetate fractions of Cliona sp., respectively. In addition, the examination of these fractions resulted in the isolation and identification of three sterols and one amino acid. The identification of the isolated compounds was confirmed by 1D and 2D NMR (Nuclear Magnetic Resonance), and MS (Mass spectrometry), and IR (Infrared) spectroscopy. The in vitro cytotoxic, antioxidant, and antimicrobial activities of the total ethanolic extract and its sub-fractions were also evaluated. Interestingly, the ethyl acetate fraction showed potent cytotoxic activity against colon (HCT-116) and human larynx carcinoma (HEP-2) cell lines with IC50 (Half-maximal Inhibitory Concentration) 6.11 ± 0.2 and 12.6 ± 0.9 µg/mL, respectively. However, the dichloromethane fraction showed strong antioxidant activity, with IC50 75.53 ± 3.41 µg/mL. Notably, the total ethanolic extract showed the strongest antibacterial activity against Staphylococcus aureus and Escherichia coli, with MIC (Minimum Inhibitory Concentration) 62.5 ± 0.82 and 125 ± 0.62 µg/mL, respectively, compared to other fractions. In conclusion, this is the first report on the secondary metabolites content and biological activities of Cliona sp. from the Red Sea, Egypt. It also highlights the need for further research on the most active fractions against various cancer cell lines and resistant bacterial and fungal strains. Cliona sp. extract and its fractions could be a potential source of novel and safe natural drugs with a wide range of medicinal and pharmaceutical applications.

Metabolomics analysis reveals the accumulation patterns of flavonoids and phenolic acids in quinoa (Chenopodium quinoa Willd.) grains of different colors

Quinoa grains are gaining increasing popularity owing to their high nutritional merits. However, only limited information is available on the metabolic profiles of quinoa grains. In this study, we determined the metabolic profiles of black, red, and white quinoa grains via an ultraperformance liquid chromatography–electrospray ionization–tandem mass spectrometry (UPLC–ESI–MS/MS)-based metabolomics. A total of 689 metabolites were identified, among which 251, 182, and 317 metabolites displayed different accumulation patterns in the three comparison groups (Black vs Red, Black vs White, and Red vs White), respectively. In particular, flavonoid and phenolic acid contents displayed considerable differences, with 22 flavonoids, 5 phenolic acids, and 1 betacyanin being differentially accumulated among the three quinoa cultivars. Additionally, correlation analysis showed that flavonoids and phenolic acids could act as betanin co-pigments in quinoa grains. In conclusion, this study provides comprehensive insights into the adequate utilization and development of novel quinoa-based functional foods.

Characterization of the WRKY Gene Family Related to Anthocyanin Biosynthesis and the Regulation Mechanism under Drought Stress and Methyl Jasmonate Treatment in Lycoris radiata.

Lycoris radiata, belonging to the Amaryllidaceae family, is a well-known Chinese traditional medicinal plant and susceptible to many stresses. WRKY proteins are one of the largest families of transcription factors (TFs) in plants and play significant functions in regulating physiological metabolisms and abiotic stress responses. The WRKY TF family has been identified and investigated in many medicinal plants, but its members and functions are not identified in L. radiata. In this study, a total of 31 L. radiata WRKY (LrWRKY) genes were identified based on the transcriptome-sequencing data. Next, the LrWRKYs were divided into three major clades (Group I-III) based on the WRKY domains. A motif analysis showed the members within same group shared a similar motif component, indicating a conservational function. Furthermore, subcellular localization analysis exhibited that most LrWRKYs were localized in the nucleus. The expression pattern of the LrWRKY genes differed across tissues and might be important for Lycoris growth and flower development. There were large differences among the LrWRKYs based on the transcriptional levels under drought stress and MeJA treatments. Moreover, a total of 18 anthocyanin components were characterized using an ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) analysis and pelargonidin-3-O-glucoside-5-O-arabinoside as well as cyanidin-3-O-sambubioside were identified as the major anthocyanin aglycones responsible for the coloration of the red petals in L. radiata. We further established a gene-to-metabolite correlation network and identified LrWRKY3 and LrWRKY27 significant association with the accumulation of pelargonidin-3-O-glucoside-5-O-arabinoside in the Lycoris red petals. These results provide an important theoretical basis for further exploring the molecular basis and regulatory mechanism of WRKY TFs in anthocyanin biosynthesis and in response to drought stress and MeJA treatment.

Transcription and Metabolism Pathways of Anthocyanin in Purple Shamrock (Oxalis triangularis A.St.-Hil.).

Anthocyanins are water-soluble pigments that can impart various colors to plants. Purple shamrock (Oxalis triangularis) possesses unique ornamental value due to its purple leaves. In this study, three anthocyanins, including malvidin 3-O-(4-O-(6-O-malonyl-glucopyranoside)-rhamnopyranosyl)-5-O-(6-O-malonyl-glucopyranoside), delphinidin-3-O-rutinoside and malvidin-3,5-di-O-glucoside, were characterized with ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS) in purple shamrock. To investigate the molecular mechanism of anthocyanin biosynthesis in green shamrock (Oxalis corymbosa) and purple shamrock, RNA-seq and qRT-PCR were performed, and the results showed that most of the anthocyanin biosynthetic and regulatory genes were up-regulated in purple shamrock. Then, dark treatment and low temperature treatment experiments in purple shamrock showed that both light and low temperature can induce the biosynthesis of anthocyanins.

Enhancement of Digestion Resistance and Glycemic Control of Corn Starch through Conjugation with Gallic Acid and Quercetin Using the Free Radical Grafting Method

The objective of this study was to synthesize different polyphenol–corn starch complexes including gallic acid–starch and quercetin–starch by conjugating corn starch with gallic acid and quercetin using the free radical grafting method. This process was effective in enhancing conjugations of starch molecules with gallic acid and quercetin (5.20 and 5.83 mg GAE/g, respectively) and imparted promising antioxidant capacity to the phenolic–starch complexes. Significant interactions between these phenolic compounds and corn starch molecules were revealed with an ultraperformance liquid chromatography electrospray ionization Q-time-of-flight mass spectrometry assay. It was revealed that significantly higher levels of resistant starch in the above gallic–starch and quercetin–starch complex samples (11.6 and 15.3 g/100 g, respectively) together with an obvious reduction in glycemic response (7.9% and 11.8%, respectively) observed over the control. Complex samples functionalized with gallic acid and quercetin have exerted modified physicochemical properties, particularly reduction in swelling ability (58.7–60.1%), breakdown viscosity (62.5–67.8%), and setback viscosity (37.7–44.5%). In sum, free radical grafting treatment could be a promising method for imparting corn starch with enhanced resistance to enzyme digestion along with changes in pasting properties for specific food applications.

Lipidomic analysis and triglyceride profiles of fish oil: Preparation through silica gel column and enzymatic treatment

A comprehensive study of lipidomic coupled with triglyceride profiles onto four fish oils was performed through ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry (UPLC-ESI-MS/MS). Overall, 1010 lipids belonging to 6 categories and 38 lipid classes were identified. Triglycerides (TGs) were the dominant component in four fish oils (40 %–99 % of total lipids), and glycerophospholipids (GPs) and sphingolipids (SLs) were another two major lipid categories in the fish oil (TG50) which prepared through silica gel column. These results revealed that enzymatic treatment has slight effect on lipid distribution but silica gel column could change the lipids composition. TGs composition of four fish oils were separated completely, and the most TG molecule in TG50 is TG(18:3_14:0_18:0), possessed 13.03 ± 5.07 % relative content, these results implied that silica gel column could protect the nature structure of TGs from destroying which may also limited to further improve eicosapentaenoic acid/docosahexaenoic acid (EPA/DHA) purity, but enzymic method was not restricted by this.

Nontarget Metabolites of Rhizomes of Edible Sacred Lotus Provide New Insights into Rhizome Browning

The “edible rhizome” variant of Nelumbo nucifera with various cultivars has a long history of use as a food in East Asia. In this study, 48 target metabolites were untargeted and identified in 212 rhizome cultivars (tropical and temperate types) using ultraperformance liquid chromatography-electrospray ionization quadrupole time-of-flight high-resolution mass spectrometry; among these, 32 compounds were newly reported in the rhizome. Combined with the browning phenotype of 212 lotus rhizomes, (epi) catechin, norarmepavine, and N-feruloyl-3-methoxytyramine were used as predominant chemical markers to separate different degrees of lotus rhizome browning. p-Coumaroyltyramine and N-trans-feruloyltyramine were selected as predominant chemical markers to investigate the differential expression between tropical and temperate lotus using principal component analysis and orthogonal partial least squares discriminant analysis. Shared and unique structure plots were used to compare the outcomes of the ecotype and browning OPLS model, showing that variation in tropical lotus rhizome browning is not obvious; this will be of great importance for genetic improvement by providing a hereditary basis.

Determination of the Oxidative Stress Biomarkers of 8-Hydroxydeoxyguanosine and Dityrosine in the Gills, Skin, Dorsal Fin, and Liver Tissue of Atlantic Salmon (Salmo salar) Parr.

Oxidative stress is a condition caused by an imbalance in the occurrence of reactive oxygen species in the cells and tissues of organisms. An ultra-performance liquid chromatography–electrospray ionization tandem mass spectrometry (UPLC–ESI–MS/MS) method was developed for the simultaneous determination of two oxidative stress biomarkers, 8-hydroxydeoxyguanosine (8OHDG) and dityrosine (DIY), in the gills, skin, dorsal fin, and liver tissue of Atlantic salmon (Salmo salar) parr. The use of target analyte-specific 13C and 15N internal standards allowed quantification of each target analyte to be performed through the standard solvent calibration curve. The relative recoveries [mean ± (relative standard deviation%)] of 8OHDG and DIY were 101 ± 11 and 104 ± 13% at a fortified concentration of 10 ng/mL (8OHDG) and 500 ng/mL (DIY), respectively, ensuring the accuracy of the extraction and quantification. The chromatographic separation was carried out using a gradient elution program with a total run time of 5 min. The limits of detection (LODs) were 0.11 and 1.37 ng/g wet weight (w.w.) for 8OHDG and DIY, respectively. To demonstrate the applicability of the developed method, it was applied in 907 tissue samples that were collected from Atlantic salmon parr individuals reared in an experimental land-based recirculating aquaculture system (RAS) treated with peracetic acid. Moreover, the possibility of using the dorsal fin as an alternative matrix for the minimally invasive assessment of oxidative stress in Atlantic salmon parr was introduced. To our knowledge, 8OHDG and DIY were used for the first time as biomarkers for biomonitoring the fish health (oxidative stress) of Atlantic salmon parr in RAS.

Lipidomic profile changes of yellow-feathered chicken meat during thermal processing based on UPLC-ESI-MS approach

In this work, ultra-performance liquid chromatography-electrospray ionization mass spectrometry (UPLC-ESI-MS) was applied to compare the lipidomics profile of chicken breast meat heated to various temperatures. A total of 445 lipids including phospholipids, diacylglycerols, triacylglycerols, glycoglycerolipids, and sphingolipids were detected in chicken muscle. Significant decreases in a list of characteristic unsaturated phospholipid species including phosphatidylcholine, phosphatidylethanolamine, phosphatidylglycerol and phosphatidylinositol were identified after heating, suggesting the occurrence of lipid oxidation, while significant increases in characteristic lysophospholipid species were found with increasing heating temperature, which were mainly derived from hydrolysis of phospholipids. Moreover, ether phospholipid and neutral lipid species exhibited remarkable changes during the heating process, and monoalk(en)yl diacylglycerol was first identified in chicken meat. The findings could contribute to the improved understanding of key lipids and biochemical reactions engaged in the heating of meat products.

Effect of fermentation stages on glucosinolate profiles in kimchi: Quantification of 14 intact glucosinolates using ultra-performance liquid chromatography-tandem mass spectrometry.

We developed and validated an ultra-performance liquid chromatography-electrospray ionization tandem mass spectrometry-based analytical method to determine intact glucosinolates in kimchi and evaluate the effects of fermentation stages on glucosinolate profiles. The developed method yielded reliable data in the kimchi matrix in terms of selectivity, matrix effect (88%-105%), linearity (coefficients of determination ≥0.9991), sensitivity (limits of quantification ≤35nmol/L), accuracy (82%-101%), and precision (≤8%). The kimchi samples contained progoitrin, sinigrin, glucoraphanin, glucoraphenin, glucoalyssin, gluconapin, glucobrassicanapin, glucobrassicin, glucoberteroin, gluconasturtiin, 4-methoxyglucobrassicin, and neoglucobrassicin, of which 4-methoxyglucobrassicin, glucobrassicanapin, and gluconapin were the major compounds. Total glucosinolate content was decreased by 31%-97% and 91-100% in the moderate-fermented and over-fermented samples, respectively, compared with that in the non-fermented samples, revealing sudden glucosinolate degradation between the moderate- and over-fermentation stages. In summary, we report an efficient analytical method to estimate kimchi glucosinolate profiles, which could be a foundation for future studies.