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Citrus peels are rich in flavonoids, and some valuable flavonoids with health benefits, such as polymethoxyflavones (PMFs), are found almost exclusively in citrus peels. While the peels usually regarded as by-product, leading to source waste. As a traditional method, drying is helpful to increase added-value of peels which can be used as medicine. However, the variations in variety and quantity of flavonoids during drying processes of citrus peel remain unknown. In this study, Guanxi honey pomelo peel investigated the effect of different drying methods on flavonoids content in citrus peels. Five drying techniques, namely, freeze-drying (FD) and hot air drying (HAD) at 30 °C, 50 °C, 70 °C and 90 °C were used employed for drying the pomelo peels and HPLC-Q-TOF-MS analysis identified 39 flavonoids changes in flavonoids across samples. FD proved to better preserve most glycosidic flavonoids. Flavonoid aglycones could be better preserved in samples of HAD at 30 ℃, 50 ℃ HAD and 90 ℃ HAD. Specifically, HAD at 30 ℃ and 50 ℃ HAD is beneficial for obtaining more valued polymethoxyflavones such as 5-hydroxy-6,7,4′-trimethoxyflavone, 5,7,8,4′-tetramethoxyflavone and 3,5,6,7,8,3′,4′-heptamethoxyflavone. The 90℃ HAD resulted in the highest content of naringenin and 5,7,8,4′-tetramethoxyflavanone. This study demonstrated the transformation characteristics of flavonoids in pomelo peel under varying drying conditions, providing benefits for comprehensive utilization of pomelo peel in extracting valued-added flavonoids. [ABSTRACT FROM AUTHOR]

Background: Sweet Basil (Ocimum basilicum L.) is regarded as a significant plant. They include a wide variety of bioactive substances, particularly phenolic substances which contribute to the plant's alleged health advantages. Aim: The objective of this study was to identify and characterize the phenolic profile of sweet basil using HPLC-Q-TOF-MS in order to evaluate its anti-inflammatory and antioxidant properties. Methods: By using standard protocols, Bioactive molecules were extracted and qualitative tests of phytochemicals were also released as well as quantitative analyses of total phenols, total flavonoids, and total hydrolysable tannins. Using HPLCQ-TOF-MS, phenolic compounds can be identified. Antioxidant and anti-inflammatory activities were studied by DPPH, FRAP, RBC membrane stabilization and BSA anti denaturation assays. Results: 30 phenolic compounds in this plant were identified by the HPLC-Q-TOF-MS analysis. Moreover, the TPC, TFC, and THTC of sweet basil was systematically assessed, and then its antioxidant and anti-inflammatory properties were evaluated using the DPPH, FRAP, RBC membrane stabilization, and BSA anti denaturation assays. Significant anti-inflammatory and antioxidant effects were also seen in the plant extracts with high phenolic, flavonoid, and tannin content. Conclusion: The results demonstrate the value of sweet basil (Ocimum basilicum L.) which may be used in the food and health industries as promising sources of phenolic chemicals. [ABSTRACT FROM AUTHOR]

Prunella vulgaris has long been used in traditional medicine and is consumed as a tea in China. Here, the total phenolic and flavonoid concentrations of plants from different geographical regions were measured. It was found that the total phenolic acid concentration ranged from 4.15 to 8.82 g of gallic acid equivalent per 100 g of dry weight (DW), and the total flavonoid concentration was 4.67–7.33 g of rutin equivalent per 100 g DW. Antioxidant activities were measured using 2,2‐diphenyl‐1‐picrylhydrazyl and 2,2′‐azino‐bis‐(3‐ethylbenzothiazoline‐6‐sulfonic acid) diammonium salt, and the results ranged from 73.47% to 94.43% and 74.54% to 93.39%, respectively, whereas α‐glucosidase inhibition was between 75.31% and 95.49%. Correlation analysis showed that the total flavonoids in P. vulgaris had superior antioxidant and anti‐α‐glucosidase activities compared to the total phenolic compounds. The active components of P. vulgaris were analyzed using high‐performance liquid chromatography quadrupole time‐of‐flight mass spectrometry combined with both classical molecular networking and feature‐based molecular networking on the Global Natural Products Social platform, identifying 32 compounds, namely 14 flavonoids, 12 phenolic compounds, and 6 other chemical components. These results could provide useful information on the use of P. vulgaris as a functional tea. [ABSTRACT FROM AUTHOR]

Li‐Zhong‐Xiao‐Pi granules (LZXP) are effective for treating gastric precancerous lesions (GPL) in traditional Chinese medicine. However, the active compounds of LZXP and their potential therapeutic mechanism in GPL remained unclarified. The purpose of this study is to investigate the chemical composition and potential targets of LZXP. Based on the accurate masses, ion fragments, and literature data, a total of 128 compounds were identified in the LZXP sample using ultra‐performance liquid chromatography and quadrupole time‐of‐flight mass spectrometry (UPLC–Q‐TOF–MS) in both positive and negative ion modes, and 28 of these compounds were exactly determined by comparison with authentic reference standards. Meanwhile, 11 typical components were quantified via UPLC during a 24 min period. The linearity, accuracy, stability and recovery of the method were all proven. Through the network pharmacological analysis, six chemicals (quercetin, 4′‐hydroxywogonin, sinensetin, 5, 7, 8, 3′, 4′‐pentamethoxyflavanone, 8‐gingerdione and quercetin) were identified as the active ingredients, and five LZXP targets (AKT1, CYP1B1, PTGS2, MMP9 and EGFR) were found to be the crucial molecules in the treatment of GPL. This study provides a systematic and applicable method for the rapid screening and identification of the chemical constituents from LZXP, and an effective understanding the mechanism of LZXP in the treatment of GPL. [ABSTRACT FROM AUTHOR]

Accurate classification and understanding of metabolite variations in Eurycoma longifolia according to source, harvesting age, and planting location are of great importance to ensure the quality and standardization of E. longifolia-based products. In this study, an untargeted metabolomic approach using high-performance liquid chromatography coupled to quadrupole-time-of-flight mass spectrometry (HPLC-Q-ToF-MS) was used to classify E. longifolia samples and to determine metabolite variations in 1-, 4-, and 11-year-old E. longifolia roots collected from different planting locations. Principal component analysis (PCA) and hierarchical clustering analysis showed clear separation between hairy root culture and E. longifolia root samples, highlighting apparent metabolite differences between these samples. Moreover, the approach successfully separated E. longifolia root samples according to their harvesting age and planting location. The PCA loading plot after varimax rotation revealed that dominant ions with strong loadings to principal component 1 were identified as canthin-6-one alkaloid and quassinoid compounds. Overall, the findings indicate that HPLC-Q-ToF-MS-based metabolomics is a powerful approach to classify and determine metabolite variations in E. longifolia samples. [ABSTRACT FROM AUTHOR]

Hemerocallis citrina Baroni [Asphodelaceae], which is traditional herbal medicine, has been widely used for treating depressive disorders in Eastern-Asia countries. However, the active compounds and corresponding mechanism of anti-depression are not yet completely clarified. In this study, the antidepressive activities of six H. citrina extracts were primarily evaluated. The results showed that the water extract of H. citrina flowers (HCW) displays significant anti-depressive activity. A total of 32 metabolites were identified from HCW by high-performance liquid chromatography/quadrupole time-offlight mass spectrometry (HPLC-Q-TOF-MS) and nuclear magnetic resonance (NMR). And then, the anti-depressive activity of the high-level compound (rutin) in HCW was also estimated. The results indicated that rutin displayed significant anti-depressive activity and was one of the main active ingredients. Finally, the anti-depressive mechanisms of HCW and rutin were investigated based on the intestinal microorganisms. The results showed that HCW and rutin increase the diversity and richness of the intestinal flora and regulate the specific intestinal microorganisms such as Bacteroides and Desulfovibrio genera in depressed mice. This work marks the first comprehensive study of the active components, anti-depressive activities and corresponding mechanisms of different H. citrina extracts, which provide a potential possibility for developing new antidepressants. [ABSTRACT FROM AUTHOR]

This study aimed to identify and quantify the primary components in lotus leaf and to explore the hypolipidemic components through spectral-effect relationships and chemometric methods. Utilizing a data-dependent acquisition-diagnostic fragment ion/characteristic neutral loss screening strategy (DFI-NLS), a reliable HPLC-Q-TOF-MS analysis was conducted, identifying 77 compounds, including 36 flavonoids, 21 alkaloids, 3 terpenoids, 11 organic acids, 4 phenols, 1 lignin and 1 unsaturated hydrocarbon. A straightforward HPLC-DAD method was developed for the simultaneous determination of seven major components in lotus leaf, and quercetin-3-O-glucuronide (Q3GA) was identified as the most abundant component. The HPLC fingerprints of 36 lotus leaf sample batches were assessed using chemometric approaches such as principal component analysis and hierarchical cluster analysis. The hypolipidemic effect of these samples was analyzed by measuring total cholesterol (TC) and total triglycerides (TG) levels in palmitic acid (PA) and oleic acid (OA)-induced lipid modeling in HepG-2 cells, employing partial least squares regression and grey relation analysis to investigate the spectral-effect relationship of the lotus leaf. The in vivo hypolipidemic effect of these compounds was assessed using an egg yolk powder-induced high-fat zebrafish model. The findings indicated that peak No.11 (Q3GA) in the chemical fingerprint was significantly associated with hypolipidemic activity, suggesting it as a potential hypolipidemic compound in lotus leaf. In summary, this study facilitates the exploration of the phytochemical compounds and their bioactive properties in the lotus leaf. [Display omitted] • Seventy-seven compounds were comprehensively identified in lotus leaf. • Flavonoids in lotus leaf exhibit significant hypolipidemic activity. • Quercituron is a compound with potent hypolipidemic activity in lotus leaf. [ABSTRACT FROM AUTHOR]

Neuraminidase inhibitors (NAIs) are the mainstay antiviral drugs against influenza infection. In this study, a ligand fishing protocol was developed to screen NAIs using neuraminidase immobilized magnetic beads (NA-MB). After verifying the feasibility of NA-MB with an artificial mixture including NA inhibitors and non-inhibitors, the developed ligand fishing protocol was applied to screen NAIs from the crude extracts of Duchesnea indica Andr. Twenty-four NA binding compounds were identified from the normal butanol (n-BuOH) extract of D. indica as potential NAIs by high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC–Q-TOF-MS) assisted with Compound Structure Identification (CSI):FingerID, including 12 ellagitannins, 4 brevifolin derivatives, 3 ellagic acid derivatives, and 4 flavonoids. Among them, 9 compounds were isolated and tested for in vitro NA inhibitory activities against NA from Clostridium perfringens, and from oseltamivir sensitive and resistant influenza A virus strains. The results indicate that compound B23 has the NA inhibitory activities in both the oseltamivir sensitive and resistant viral NA, with half maximal inhibitory concentration (IC50) values of 197.9 and 125.4 μmol/L, respectively. Moreover, B23 can obviously reduce the replication of oseltamivir sensitive and resistant viruses in Madin–Darby canine kidney (MDCK) cells at the concentrations of 40 and 200 μmol/L.

Introduction: Dandelion (Taraxacum mongolicum Hand.‐Mazz.) is a perennial herb with diverse pharmacological effects. The development and utilization of dandelion have attracted much attention. Objectives: Our aims were to provide a reference basis for the identification of the origin of dandelions and to study the influence of their origin on their quality. Methods High‐performance liquid chromatography coupled with quadrupole time‐of‐flight mass spectrometry was used to analyze metabolites from dandelions from four different geographical regions in China, namely Gansu, Henan, Shanxi, and Jiangsu. Metabolite analysis was performed using orthogonal partial least‐squares discriminant analysis, and to identify potential metabolic pathways, MBRole was used to perform Kyoto Encyclopedia of Genes and Genomes (KEGG) pathway enrichment analysis. Results: Principal component analysis revealed that the chemical components of dandelions sampled from the four regions showed noticeable differences. Twenty‐six, six, six, eight, eight, and fifteen differentially produced metabolites were identified upon comparison between Gansu and Jiangsu, Gansu and Shanxi, Gansu and Henan, Henan and Shanxi, Henan and Jiangsu, and Shanxi and Jiangsu, respectively. These differentially produced metabolites were mainly phenolic compounds. Further, KEGG pathway enrichment analysis showed that the main metabolic pathways involved were biosynthesis of phenylpropanoids and flavonoids. Conclusion: The methods reported herein can be used to identify the origin of dandelions; moreover, our results can serve as a reference basis for future studies. Dandelion is distributed in many places and has been widely used in recent years. In this paper, an analysis method based on LC‐MS/MS was proposed to identify the origin of dandelions and phenolic compounds were found to be the main different metabolites in dandelions for different geographical regions. The results of KEGG enrichment analysis found that different geographical regions environmental stresses contribute to differences in dandelion quality through affect the biosynthesis of phenylpropanoids and flavonoids. [ABSTRACT FROM AUTHOR]

Allergic diseases are a significant public health problem worldwide. Traditional Chinese medicines (TCMs) with reported anti-allergy effects may be important sources for the development of new anti-allergy drugs. Thus, establishing an analytical method that can simultaneously identify and screen anti-allergic compounds in TCMs is important. The increased concentrations of intracellular calcium ions resulting in mast cell degranulation releasing active mediators play a key role in allergic diseases, which can be used as a potential index to identify anti-allergic herbs and compounds. In this study, we provide a new strategy that was applied to screening natural anti-allergic compounds based on fluorescence calcium ion (Ca2+) fluctuation integrated with cell extract and high-performance liquid chromatography–mass spectrometry (HPLC–MS). A low-cost, convenient fluorescence detection Ca2+ signaling method was established and successfully applied to identify three herbs. Then, the method was integrated with biospecific cell fishing and HPLC–MS to screen potential active components that have the effect of stabilizing the cell membrane of rat basophilic leukemia granulocytes (RBL-2H3). Seven components, namely, albiflorin and paeoniflorin from Radix Paeoniae Alba, ononin and formononetin from Radix Astragali, cimifugin, 4′-O-β-D-glucosyl-5-O-methylvisamminol, and prim-O-glucosylcimifugin from Radix Saposhnikoviae were fished. These seven compounds have the effect of inhibiting cell Ca2+ influx. 4′-O-β-D-Glucosyl-5-O-methylvisamminol, prim-O-glucosylcimifugin, paeoniflorin, ononin, and formononetin significantly inhibit the release of β-hexosaminidase, which is equivalent to the positive drug. In conclusion, the integrated strategy of fluorescence detection calcium ion kinetic method binding with biospecific cell fishing was an effective mode to identify and screen natural anti-allergic compounds. [ABSTRACT FROM AUTHOR]

Copyright of Tobacco Science & Technology is the property of Tobacco Science & Technology and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Neuraminidase inhibitors (NAIs) are the mainstay antiviral drugs against influenza infection. In this study, a ligand fishing protocol was developed to screen NAIs using neuraminidase immobilized magnetic beads (NA-MB). After verifying the feasibility of NA-MB with an artificial mixture including NA inhibitors and non-inhibitors, the developed ligand fishing protocol was applied to screen NAIs from the crude extracts of Duchesnea indica Andr. Twenty-four NA binding compounds were identified from the normal butanol (n -BuOH) extract of D. indica as potential NAIs by high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC–Q-TOF-MS) assisted with Compound Structure Identification (CSI):FingerID, including 12 ellagitannins, 4 brevifolin derivatives, 3 ellagic acid derivatives, and 4 flavonoids. Among them, 9 compounds were isolated and tested for in vitro NA inhibitory activities against NA from Clostridium perfringens , and from oseltamivir sensitive and resistant influenza A virus strains. The results indicate that compound B23 has the NA inhibitory activities in both the oseltamivir sensitive and resistant viral NA, with half maximal inhibitory concentration (IC 50) values of 197.9 and 125.4 μmol/L, respectively. Moreover, B23 can obviously reduce the replication of oseltamivir sensitive and resistant viruses in Madin–Darby canine kidney (MDCK) cells at the concentrations of 40 and 200 μmol/L. An efficient neuraminidase ligand fishing protocol was developed and verified to rapidly screen the neuraminidase inhibitors (NAIs) from natural sources. Twenty-four potential neuraminidase inhibitors were identified from Duchesnea indica as potential NAIs by HPLC–Q-TOF-MS. One compound can inhibit neuraminidase activities in both the oseltamivir sensitive and resistant virus strains. Image 1 • An efficient ligand fishing protocol was developed to rapidly screen the neuraminidase inhibitors from natural sources. • 24 potential neuraminidase inhibitors were identified from Duchesnea indica as potential NAIs by HPLC-Q-TOF-MS. • One compound can inhibit neuraminidase activities in both the oseltamivir sensitive and resistant virus strains. [ABSTRACT FROM AUTHOR]

A novel peptide, Cys-Trp-Cys (CWC), which firstly isolated from Guojing Baijiu was qualitative and quantitative studied by high-performance liquid chromatography and quadrupole-time-of-flight-mass spectrometry (HPLC- Q-TOF-MS) with a concentration of 11.06 ± 0.34 μg/L (P > 0.05). The antioxidant activity of the peptide was evaluated by the HepG2 cell model induced by 2, 2′-azobis (2-methyl propanimidamidine) dihydrochloride (AAPH) and in vitro chemical assays, including (1,1-diphenyl- 2-picrylhydrazyl radical 2,2-diphenyl- 1-(2,4,6-trinitrophenyl) hydrazyl (DPPH), 2,2'-azinobis-(3-ethylbenzthiazoline- 6-sulphonate) (ABTS), oxygen radical absorbance capacity, reducing power, and metal chelation assays. The results showed that CWC exhibited stronger antioxidant activity than Trolox in the ABTS assay. Furthermore, CWC inhibited AAPH-induced oxidative stress in HepG2 cells with a dose-dependent manner. Pretreatment of the cells with CWC (1, 2, and 4 mg/mL) caused the strong scavenging activities on the intracellular reactive oxygen species and a marked decrease in the reduced malondialdehyde (MDA). In addition, pretreatment with CWC prevented significantly the activities decrease in glutathione peroxidase (GSH-Px), superoxide dismutase (SOD), and catalase (CAT) induced by AAPH. CWC had strong antioxidant activity mainly due to its Cys residue containing a thiol group (–SH). These findings indicated that CWC was a potent natural antioxidant in Baijiu, which would be important for deeply understanding the relationship between the health and Baijiu. [ABSTRACT FROM AUTHOR]

Reduced nitrogen-containing organic compounds (NOCs) in aerosols play a crucial role in altering their light-absorption properties, thereby impacting regional haze and climate. Due to the low concentration levels of individual NOCs in the air, the utilization of accurate detection and quantification technologies becomes essential. For the first time, this study investigated the diurnal variation, chemical characteristics, and potential formation pathways of NOCs in urban ambient aerosols in Shanghai using a versatile aerosol concentration enrichment system (VACES) coupled with HPLC-Q-TOF-MS. The results showed that NOCs accounted over 60% of identified components of urban organic aerosols, with O/N < 3 compounds being the major contributors (>70%). The predominance of the positive ionization mode suggested the prevalence of reduced NOCs. Higher relative intensities and number fractions of NOCs were observed during nighttime, while CHO compounds showed an opposite trend. Notably, a positive correlation between the intensity of NOCs and ammonium during the nighttime was observed, suggesting that the reaction of ammonium to form imines may be a potential pathway for the formation of reduced NOCs during the nighttime. Seven prevalent types of reduced NOCs in autumn and winter were identified and characterized by an enrichment of CH 2 long-chain homologues. These NOCs included alkyl, cyclic, and aromatic amides in CHON compounds, as well as heterocyclic or cyclic amines and aniline homologue series in CHN compounds, which were associated with anthropogenic activities and may be capable of forming light-absorbing chromophores or posing harm to human health. The findings highlight the significant contributions of both primary emissions and ammonium chemistry, particularly amination processes, to the pollution of reduced NOCs in Shanghai's atmosphere.

A rapid method based on solvent extraction followed by direct injection in liquid chromatography-quadrupole-time-of-flight-mass spectrometry (LC-Q-TOF-MS) was developed for the targeted and suspect screening of contaminants in the soft tissues of the pearl oyster Pinctada imbricata radiata. The quantification method was first validated for the targeted analysis of 21 contaminants including some pharmaceutically active compounds, with the relative recoveries ranging from 88 to 123%, and method detection limits generally below 1 ng g−1 on the wet weight (ww) basis. This targeted analysis method was then applied to oyster samples collected around the Qatari coast between 2017/2018, and none of the 21 compounds were detected in these samples. The post-acquisition data treatment based on the accurate mass measurement in both full MS scan and All Ions MS/MS was further used for mining other contaminants in oyster extracts, as well as 21 targeted compounds spiked in oyster extracts (suspect screening). The 21 spiked compounds were identified successfully and the estimated limit of identification for the individual 21 compounds ranged from 0.5 to 117 ng g−1 ww of oyster tissues. A phthalate, di(2-ethylhexyl) phthalate (DEHP) was identified to be present in oyster extracts from 2018 batches, at a concentration level significantly higher than that in procedure blanks. These results confirmed that high resolution MS data obtained using the targeted method can be exploited through suspect screening workflows to identify contaminants in the tissues of bioindicator mollusks. However, a number of false identifications could be obtained and future work will be on improving the success rate of the correct identifications using this workflow. Image 1 • a method allowed for the targeted and suspect screenings of contaminants in pearl oysters. • The method was validated for the targeted analysis of 21 contaminants (incl. pharmaceuticals). • This method could identify contaminants through suspect screening. • The estimated limit of identification for the 21 compounds ranged from 0.5 to 117 ng g−1 of oyster tissues. An analytical method was developed for the target and suspect screenings of contaminants in pearl oyster tissues. [ABSTRACT FROM AUTHOR]

The targeted analysis of veterinary drug residues in honey traditionally involves a series of extraction and purification steps prior to quantification with high performance liquid chromatography coupled to high resolution or tandem mass spectrometry. These steps, designed to separate the target analytes from interferences, are generally time-consuming and costly. In addition, traditional cleanup steps are likely to eliminate other compounds whose analysis could prove decisive in current or future assessment of the honey sample. Alternatively, direct injection without complex sample preparation steps has been introduced for the fast analysis of trace compounds in environmental and food matrices. The aim of this study was to develop a rapid method for the targeted analysis of 7 key veterinary drug residues in honey based on direct injection high performance liquid chromatography coupled to quadrupole time-of-flight, while simultaneously recording dataindependent MS/MS (e.g. All Ions MS/MS data) for future re-examination of the data for other purposes. The new method allowed for the detection of the target residues at levels approximately 20-100 times lower than current regulatory limits, for a total analysis time of about 45 min. The recoveries (103-119%), the linearity (R ≥ 0.996) and the repeatability (RSD ≤ 7%) were satisfactory. The method was then applied to 35 honey samples from the Canadian market. Residues of tylosin A, tylosin B, sulfamethazine and sulfadimethoxine were detected in 6, 9, 6 and 23% of the samples respectively, at levels below the regulatory limits in Canada. The possibility of adding a hydrolysis step to study sulfonamides in honey was tested, which provided good results for this family of compounds but lead to degradation of some of the other analytes. Finally, the non-targeted identification of several compounds was demonstrated as a proof of concept of future re-examination of All Ions MS/MS data. This paper illustrates the capacity of this novel method to combine targeted and non-targeted screening of chemical residues in honey. [ABSTRACT FROM AUTHOR]

• Characterization, quantitation and evaluation of cardiac glycosides were reported. • The inhibition of Na+,K+-ATPase activity was measured. • Enzyme kinetics and molecular docking were determined. Streblus asper Lour. (Moraceae) is a medicinal plant in Asian countries including India and Thailand, possessing activities of anti-tumor, anti-allergy, anti-parasitic and anti-bacterial. In this paper, characterization, quantitation and similarity evaluation of cardiac glycosides in different parts of S. asper were investigated by HPLC-Q-TOF-MS and chemometric methods. Then, the inhibition of Na+,K+-ATPase activity by the compounds isolated from S. asper was measured. Meanwhile, enzyme kinetics and molecular docking were determined to exhibit the combination modes between cardiac glycosides and Na+,K+-ATPase. As a result, twenty peaks of cardiac glycosides were assigned. Strophanthidin-3- O - α - l -rhamnopyranosyl-(1 → 4)-6-deoxy- β - d -allopyranoside (1), glucostrebloside (2), strebloside (4) and mansonin (8) with a significant activity of inhibiting Na+,K+-ATPase (IC 50 7.55–13.60 μM) were chosen for the determination of enzyme kinetics, exhibiting anticompetitive inhibitory characteristics towards Na+,K+-ATPase. Compound 4 could reasonably bind to the active sites of Na+,K+-ATPase, proved by molecular docking. Furthermore, the contents of the major compounds in four different parts of S. asper were extremely different, analyzed by chemometric methods, similarity analysis and principle compounds analysis. All these findings indicated that the contents of major compounds in different parts of S. asper were extremely different with a significant activity of inhibiting Na+,K+-ATPase, providing a reference for determination of effective part and administered dosage. The combination modes between cardiac glycosides and Na+,K+-ATPase were also revealed by enzyme kinetics and molecular docking, which provided a basis for further study of pharmacological activity. [ABSTRACT FROM AUTHOR]

Abstract The small molecules in Chinese Baijiu have been widely reported, but there is little information on peptides since their low concentrations. A tetrapeptide, Asp-Arg-Ala-Arg (DRAR), was newly identified from Jingzhi Sesame flavor-type Baijiu (SFTB) by high-performance liquid chromatography and quadrupole-time-of-flight-mass spectrometry (HPLC-Q-TOF-MS) with a concentration of 13.159 ± 0.202 μg/L (P > 0.05). Interactions between DRAR and volatile compounds were characterized using headspace solid-phase micro-extraction coupled with gas chromatography–mass spectrometry (HS-SPME-GC–MS), and the results indicated that DRAR could suppress the volatility of aroma compounds by 0.09–39.02 %, especially with respect to esters and alcohols. The involved binding modes of DRAR with esters or alcohols in 46% ethanol/water solutions (v/v) were respectively determined by ultraviolet (UV) absorption spectroscopy. According to the Van't Hoff equation, the thermodynamic parameters (for DRAR - esters complex, ΔH = −34.7 KJ mol−1, ΔS = −66.4 J mol−1 K−1 and for DRAR - alcohols complex, ΔH = −40.8 KJ mol−1, ΔS = −91.8 J mol−1 K−1) indicated that hydrogen bonds and van der Waals forces played major roles in stabilizing the DRAR-esters and DRAR-alcohols complexes. This study will help us to further understand the interaction mechanisms between aroma compounds and peptides, and the important role of peptides on the quality of Chinese Baijiu. Graphical abstract DRAR identified from Chinese Sesame flavor-type Baijiu selectively effect the aroma. Unlabelled Image Highlights • A new tetrapeptide (Asp-Arg-Ala-Arg, DRAR) was separated from Jingzhi Baijiu. • The chemical structure of DRAR was characterized with HPLC-Q-TOF-MS. • Hydrogen bonds and van der Waals forces play major roles in stabilizing the DRAR-esters and DRAR-alcohols complexes. [ABSTRACT FROM AUTHOR]

[Display omitted] • Resins are used for purification of flavonoids in plants. • Radix Pueraria Lobata is used as herbal remedies. • Flavonoids are secondary metabolites with several beneficial health effects. • Desorption ratio and the physical properties are used to select the resin for flavonoid separation. • HPLC-TOF-MS is used to identify flavonoids from Radix Pueraria Lobata. A systematic investigation was conducted on the adsorption and desorption properties of macroporous resins including D101, ADS7, HPD600, XAD2 and HPD100 for flavonoids of Radix Pueraria Lobata. Based on the results of the adsorption capacity, desorption ratio, and physical properties of the investigated resins, ADS7 was selected for the purification of flavonoids in this study. On the basis of the correlation coefficients, the experimental results fitted the pseudo-second-order model compared to the pseudo-first model. The separation parameters of the RPL flavonoids were optimised through dynamic adsorption/desorption experiments with a column packed with ADS7. The breakthrough point was found at 30 mL of RPL flavonoids solution, while at 105 mL of 60 % ethanol, the flavonoids were completely desorbed. Furthermore, the total flavonoid content was 3.16 mg/g. HPLC-Q-TOF-MS analysis helped identify five isoflavones, including puerarin, 3′-methoxy puerarin, daidzin, 3′-hydroxy puerarin and daidzein from radix pueraria Lobata. [ABSTRACT FROM AUTHOR]

The aim of the present study was to determine the composition, antiradical and antimicrobial activity of fruits, leaves and roots of an underestimated species of barberry—Berberis iliensis—growing in Kazakhstan. Particular attention was paid to the determination of the composition of its extracts by high-performance liquid chromatography coupled with mass spectrometry (HPLC-ESI-Q-TOF-MS) analysis. As a result of the chromatographic and spectrometric study 33 secondary metabolites from the groups of phenolic acids and their esters, flavonoids, alkaloids and organic acids were identified and 15 of them—quantified. The isomers of caffeoyl-glucaric acid, caffeic acid derivatives, isoquercetin, berberine and jatrorrhizine were the most abundant components of the tested extracts. The antiradical activity tests were performed by 2,2-diphenyl-1-picrylhydrazyl (DPPH) and Folin-Ciocalteu assays on four types of extracts (water, ethanol, ethanol-water 7:3 v/v, ethanol-water 1:1 v/v) from the three organs of the plant. The highest antiradical potential (IC50 = 80 ± 6.36 µg/mL) and phenolic content (440 ± 17.1 mg gallic acid equivalents/L) was calculated for ethanol- water (1:1 v/v) extracts from the leaves and could be influenced by the abundant presence of simple phenolic acids, flavonoids and glucaric acid esters. Among reference microorganisms, M. luteus, S. epidermidis, some S. aureus and B. cereus belonging to Gram-positive bacteria and yeasts from Candida species were the most sensitive to roots extract that was found the most active among the studied samples. The results of the study classify Berberis iliensis as a strong antioxidant agent and as a plant with an antimicrobial potential.

Aurantii fructus (AF) is a traditional Chinese medicine that has been used to improve gastrointestinal motility disorders for over a thousand years, but there is no exhaustive identification of the basic chemical components and comprehensive quality control of this herb. In this study, high-performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (HPLC-Q-TOF-MS) and gas chromatography coupled mass spectrometry (GC-MS) were employed to identify the basic chemical compounds, and high-performance liquid chromatography (HPLC) was developed to determine the major biochemical markers from AF extract. There were 104 compounds belonging to eight structure types, including 13 amino acids or peptides, seven alkaloids, 18 flavanones, 14 flavones, 15 polymethoxyflavonoids, six triterpenoids, nine coumarins, and 18 volatile oils, as well as four other compounds that were systematically identified as the basic components from AF, and among them, 41 compounds were reported for the first time. Twelve bioactive ingredients were chosen as the benchmark markers to evaluate the quality of AF. The analysis was completed with a gradient elution at a flow rate of 0.7 mL/min within 55 min. This efficient method was validated showing good linearity, precision, stability, repeatability and recovery. Furthermore, the method was successfully applied to the simultaneous determination of 12 chemical markers in different samples of AF. This study could be applied to the identification of multiple bioactive substances and improve the quality control of AF. [ABSTRACT FROM AUTHOR]

The present study was designed to develop a practical strategy to tackle the problem of lacking standard compounds and limited references for identifying structure-related compounds in Streptocaulon griffithii Hook. f., especially those in trace concentrations, with a focus on antitumor activity. The cardiac glycosides (CGs)-enriched part was determined using in vitro bioactive assays in three cancer cell lines and then isolated using macroporous resins. The MS and MS/MS data were acquired using a high performance liquid chromatography coupled with hybrid quadrupole-time of flight (HPLC-Q-TOF-MS) system. To acquire data of trace compound in the extract, a multiple segment program was applied to modify the HPLC-Q-TOF-MS method. A mass defect filter (MDF) approach was employed to make a primary MS data filtration. Utilizing a MATLAB program, the redundant peaks obtained by imprecise MDF template calculated with limited references were excluded by fragment ion classification, which was based on the ion occurrence number in the MDF-filtered total ion chromatograms (TIC). Additionally, the complete cleavage pathways of CG aglycones were proposed to assist the structural identification of 29 common fragment ions (CFIs, ion occurrence number ≥ 5) and diagnostic fragment ions (DFIs, ion occurrence number < 5). As a result, 30 CGs were filtered out from the MDF results, among which 23 were identified. This newly developed strategy may provide a rapid and effective tool for identifying structure-related compounds in herbal medicines. [ABSTRACT FROM AUTHOR]

Copyright of Shipin Kexue/ Food Science is the property of Food Science Editorial Department and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Bitter orange, Citrus aurantium L. var. amara (CAVA), is an important crop and its flowers and fruits are widely used in China as a food spice, as well as in traditional Chinese medicine, due to its health-promoting properties. The secondary metabolites that are present in plant-derived foods or medicines are, in part, responsible for the health benefits and desirable flavor profiles. Nevertheless, detailed information about the bioactive ingredients in CAVA is scarce. Therefore, this study was aimed at exploring the phytochemicals of CAVA by high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS). Here, a systematic screening method combined with HPLC-Q-TOF-MS was presented. This technique was used to systematically screen metabolites, primarily from the complex matrix of CAVA, and to identify these compounds by their exact masses, characteristic fragment ions, and fragmentation behaviors. A total of 295 metabolites were screened by the screening method and 89 phytochemicals were identified in the flowers, fruits, roots, leaves, and branches of CAVA. For the first time, 69 phytochemicals (flavonoids, alkaloids, terpenoids, etc.) were reported from CAVA. The results highlight the importance of CAVA as a source of secondary metabolites in the food, medicine, and nutraceutical industries.

Cyclocarya paliurus is an edible and medicinal plant containing various bioactive components with significant health benefits. A combinative method using high-performance liquid chromatography (HPLC) fingerprint and quantitative analysis was developed and successfully applied for characterization and quality evaluation of C. paliurus leaves collected from 18 geographical locations of China. For the fingerprint analysis, 21 common peaks were observed among the 18 samples, and these peaks were identified by high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS), while a simultaneous quantification of 16 markers was conducted to interpret the variations of contents of these bioactive compounds among the C. paliurus leaves from different geographical locations. Quantification results showed that the contents of these sixteen investigated compounds varied greatly among the leaves from different locations. The developed new method would be a valuable reference for further study and development of this bioactive plant. [ABSTRACT FROM AUTHOR]

High performance liquid chromatography coupled with quadruple-time-of-flight mass spectrometry (HPLC-Q-TOF-MS) method was developed for analyzing the hydrolytic mixtures of ginsenoside R in acidic conditions (pH 3). Three catalysts, a heteropolyacid (HSiWO, SiW for short), its complex with γ-CD (SiW/γ-CD for short) and formic acid, were used for comparison. The chemical transformation products were identified based on the accurate mass measurement and the fragment ions obtained from tandem mass spectrometry. It was concluded that the catalytic efficiency of SiW (≈SiW/γ-CD) is ca. 410 times higher than that of formic acid, thus becoming the most efficient catalyst for chemical transformations of ginsenosides. [ABSTRACT FROM AUTHOR]

The fruits of Siraitia grosvenorii are considered to be health-promoting because of the diversity of their bioactive ingredients. In the present study, a screening method, using high-performance liquid chromatography/quadrupole-time-of-flight mass spectrometry (HPLC-Q-TOF-MS) combined with a screening strategy, has been established. The technology was used to systematically screening the targeted metabolites, primarily from the complex matrix of S. grosvenorii . The compounds were then identified by their exact masses and characteristic fragment ions, in comparison with the fragmentation behaviors of 19 references. Finally, 122 compounds, including 53 flavonols and flavonol glycosides, 59 triterpene glycosides and 10 siraitic acid glycosides, were screened and identified in 10-, 50- and 80-day fruits, roots, stems and leaves of S. grosvenorii . 98 of them were reported for the first time. Additionally, the distribution of all identified components in different parts of the plant was determined and metabolic networks for flavonol and triterpene glycosides were proposed. [ABSTRACT FROM AUTHOR]

Ursodeoxycholic acid has gained increasing attention due to its recent discovery of the preventive effect on SARS-CoV-2 infection. Ursodeoxycholic acid has been included in various pharmacopoeias as an old drug, and the latest European Pharmacopoeia lists nine potential related substances (impurities A∼I). However, existing methods in pharmacopoeias and literature can only quantify up to five of these impurities simultaneously, and the sensitivity is inadequate, as the impurities are isomers or cholic acid analogues lacking chromophores. Herein, a novel gradient RP-HPLC method coupled to charged aerosol detection (CAD) was developed and validated for the simultaneous separation and quantification of the nine impurities in ursodeoxycholic acid. The method proved sensitive and allowed the quantification of the impurities as low as 0.02 %. Relative correction factors of the nine impurities were all within the range of 0.8–1.2 in the gradient mode by optimizing chromatographic conditions and CAD parameters. In addition, this RP-HPLC method is fully compatible with LC-MS due to the volatile additives and high percentage of the organic phase, which can be directly used for the identification of impurities. The newly developed HPLC-CAD method was successfully applied to commercial bulk drug samples, and two unknown impurities were identified by HPLC-Q-TOF-MS. The effect of CAD parameters on the linearity and correction factors was also discussed in this study. Overall, the established HPLC-CAD method can improve the methods in current pharmacopoeias and literature and contributes to understanding the impurity profile for process improvement. [Display omitted] • Separation of all nine specified impurities of ursodiol by a single method. • HPLC with charged aerosol detector to detect impurities for lack of chromophores. • Method proved sensitive and correction factors of nine impurities were all 0.8–1.2. • Method is compatible with LC-MS and two unknown impurities were identified. • Overcoming the deficiency of existing methods in pharmacopoeias and literature. [ABSTRACT FROM AUTHOR]

Yihuang decoction (YHD) is one of the most famous formulas in tradition Chinese medicine (TCM) and has been clinically used for treatment of vaginitis, pelvic inflammation and other gynecological diseases for hundreds of years. However, its chemical composition remains unclear. In this study, high performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS) was employed for its chemical profiling investigation. As a result, 90 components were chemically defined, including 23 alkaloids, 14 organic acids, 3 phenylethanoid glycosides, 4 iridoid glycosides, 5 terpenoid lactones, 10 flavonoids, 8 nucleobases and nucleosides, 12 amino acids, and 11 other compounds. In addition, 8 representative compounds (acteoside, allantoin, berberine, 4- O -feruloylquinic acid, 5- O -feruloylquinic acid, gallic acid, geniposidic acid, and phellodendrine) were simultaneously determined in 10 batches of YHD samples by HPLC with a diode array detector (HPLC-DAD). For all the analytes, their calibration curves showed good linearity (R2 >0.9990) within the test ranges. RSDs of precision, repeatability and stability test were all below 3.50%. The overall recoveries ranged from 93.63% to 105.02%, with RSDs less than 3.50%. This study is supposed to exhibit a comprehensive chemical profiling of YHD and to provide some strong basis for quality control and even for action mechanism of this ancient classical prescription. [Display omitted] • The chemical profiling of YHD was elucidated by HPLC-Q-TOF-MS. • Totally 90 compounds have been identified in YHD. • 8 representative compounds in 10 batches of YHD were simultaneously quantified by HPLC-DAD. [ABSTRACT FROM AUTHOR]

Tinospora cordifolia ( Guduchi Sawras ) though has been clearly demonstrated in literature for its hypolipidemic and anti-alcoholism properties but its anti-hyperlipidemia mechanistic approach is still missing. Moreover, its direct implication with alcohol induced hyperlipidemia has also not been reported till date. In order to explore the answers of these questions, phytochemicals of Tinospora cordifolia water extract “ Guduchi Sawras ” (GS) was analyzed using HPLC-Q-TOF-MS. On the basis of relative peak volumes 110 compounds were selected and identified in GS. Besides that, protein targets of most abundant compounds present in GS were fetched from ChEMBL and protein interaction network (PIN) was constructed. GO enrichment analysis showed that GS targets various pathways including dopamine metabolism, cAMP-dependent signaling pathway, and glycolytic process. Biological processes obtained via PIN were correlated with hyperlipidemia markers and dopamine metabolism in moderate alcohol consumers (n = 25) and healthy volunteers (n = 27) of age 41 ± 3.8 years. Metabolic analysis demonstrated the increased serotonin (1.9-fold) and decreased dopamine (−2.3-fold) levels in alcoholics. Further data analysis revealed a significant increase in urinary BCAAs (>2.0-fold), pantothenic acid (1.8-fold), carnitines (>2-fold) levels, and decrease in PPARα activation markers levels i.e. nicotinamide-1-oxide (−1.7-fold), and N -methylnicotinamide (−1.6-fold) in alcoholics. Biochemical analysis showed the increased AST/ALT ratio (1.91), along with triglycerides (20%), and MDA (34%) and GSH (56%) levels in alcoholics. GS treatment significantly reverted the most of the discussed metabolites levels (p < 0.05) and enzymes activities (p < 0.05) in alcoholics. The data depict that moderate chronic alcohol consumption lead to hyperlipidemia and oxidative burden; whereas GS treatment ameliorates hyperlipidemia by decreasing oxidative stress, activating PPARα, CREB and SREBP-1 through stimulation of dopamine D1 receptors mediated signalling molecules i.e. cAMP and protein kinase A. [ABSTRACT FROM AUTHOR]

Zibu Piyin recipe (ZBPYR), a traditional Chinese medicine formula, is used for curing dementia caused by diabetes. For quality control of ZBPYR, fingerprint analysis and qualitative analysis using high-performance liquid chromatography (HPLC) with a diode-array detector, and confirmation using HPLC coupled with electrospray ionisation quadrupole time-of-flight tandem mass spectrometry (HPLC-Q-TOF-MS) were undertaken. HPLC fingerprint consisting of 34 common peaks was developed among 10 batches of ZBPYR, in which 7 common peaks were identified in comparison with the authentic standards and detected simultaneously. Furthermore, these seven compounds were verified by HPLC-Q-TOF-MS methods. The method can be applied to the quality control of ZBPYR. [ABSTRACT FROM AUTHOR]

A high-performance liquid chromatography (HPLC) method has been developed for the determination of related substances in egg yolk lecithin. Chromatographic separation was achieved using a gradient elution on a Waters Xbridge HILIC column maintained at 35 ℃. Mobile phase A was composed of water-acetonitrile (80:20, v/v, containing 5 mM ammonium acetate), and mobile phase B was composed of acetonitrile. Analytes were monitored by a charged aerosol detector (CAD) at 50 ℃. The novel HPLC-CAD method was selective and sensitive for the determination of related substances in egg yolk lecithin in its commercial bulk batches. It was also successfully validated by the International Council for Harmonisation (ICH) guidelines. The method will be a renewal of an old Chinese Pharmacopoeia method (2020 edition). Moreover, quadrupole time-of-flight mass spectrometry (Q-TOF-MS) was integrated with HPLC to investigate phospholipid species in egg yolk lecithin. This work provides comprehensive composition profiles of egg yolk lecithin, thereby accelerating the quality control, development, and application of egg yolk lecithin. [Display omitted] • Determination of related substances in egg yolk lecithin was developed and validated with HPLC-CAD. • In the profile of egg yolk lecithin, 121 phospholipid molecules were identified using HPLC-Q-TOF-MS. • This proposed method is selective, efficient, sensitive, and QC-friendly for routine analysis of related substances in egg yolk lecithin. [ABSTRACT FROM AUTHOR]

Timosaponin AIII, a major saponin found in Anemarrhena asphodeloides Bge., exhibits a wide spectrum of bioactivities. It is believed that it may be further developed into a promising new drug. To better understand the pharmacological activities of the component, the investigation of its in vivo and in vitro metabolism was necessary. In this study, the metabolic profile of timosaponin AIII was investigated using liquid chromatography-mass spectrometric (LC/MS) techniques. Two different types of mass spectrometers-aquadrupole time-of-flight (Q-TOF) mass spectrometer and hybrid quadrupole/linear ion trap (Q-TRAP) mass spectrometer were employed to acquire structural information on timosaponin AIII metabolites. Plasma, bile, urine and feces were collected from rats after a single oral dose of 400 mg/kg of water solution. A total of 19 metabolites were detected and tentatively identified based on the mass spectral fragmentation patterns, elution order or confirmed using available reference standard. Two metabolites were detected after incubating with rat liver microsomal. What’s more, we isolated sarsasapogenin from the collection of urine samples after timosaponin AIII (5.0 g) giving orally to 20 rats at a dose of 150.0 mg/kg in an interval of 7 days. The present study provided important information about the metabolism of timosaponin AIII which will be helpful for fully understanding the mechanism of this compound’s action. [ABSTRACT FROM AUTHOR]

Barleria grandiflora Dalz. (Acanthaceae) is being used in India to treat different types of disorders including skin infections. Therefore, there are good possibilities to find antifungal compounds in its extracts with novel mechanism of action. The main objectives of the present study were to evaluate the antifungal activity of plant extracts and to study its effects on metabolic pathways of A. fumigatus. The microbroth dilution assay was used to explore antifungal activity and MIC of various extracts. Metabolic profiles of control and treated cultures were collected from Q-TOF-MS interfaced with HPLC. Affected metabolic pathways of A. fumigatus after the treatment were analyzed by discrimination analysis of mass data. Antifungal activities were observed in hot and cold water extracts of the plant. Hot water extract of B. grandiflora showed significant activity against tested fungi in the range 0.625-1.25 mg/mL. Partial least discrimination analysis revealed that the hot water plant extract downregulated amino acid, glyoxylate pathway, and methylcitrate pathways at the same time due to the synergistic effects of secondary metabolites. Hot water extract also downregulated several other metabolic pathways unique to fungi indicating its specific activity toward fungi. B. grandiflora showed promising antifungal activity which can further be exploited by identification of active compounds, to inhibit the specific fungal pathways and development of novel therapeutic antifungal drugs. [ABSTRACT FROM AUTHOR]

Ding-Zhi-Xiao-Wan (DZXW) is a famous traditional Chinese medicine (TCM) formula, which is composed of four herbs, Ginseng Radix, Poria, Polygala Radix and Acori Tatarinowii Rhizoma. It has been popularly used for the treatment of emotional disease, like Alzheimer's disease, Parkinson's disease, depression, anxiety, forgetfulness and neurasthenia. In this research, a high-performance liquid chromatography coupled with ion-trap tandem mass spectrometry (HPLC-IT-MSn) method along with a high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MSn) method in negative ion mode was established to investigate the major constitutions in DZXW. The extracts were prepared by ultra-sonication in ethyl acetate, n-butanol, 95% ethanol and deionized water sequentially as well as in deionized water directly. A Kromasil C18 column was used to separate the extracts of DZXW. Acetonitrile and 0.1% aqueous formic acid (V/V) were used as the mobile phase. A total of 64 components were characterized, including 16 triterpenoids, 14 Polygala saponins, 10 oligosaccharide esters, 6 sucrose esters, 2 xanthone C-glycosides and 16 ginsenosides. [ABSTRACT FROM AUTHOR]

Bread is one of the most widely consumed foods. Its impact on human health is currently of special interest for researchers. We aimed to identify biomarkers of bread consumption by applying a nutrimetabolomic approach to a free-living population. An untargeted HPLC-q-TOF-MS and multivariate analysis was applied to human urine from 155 subjects stratified by habitual bread consumption in three groups: non-consumers of bread ( n = 56), white-bread consumers ( n = 48) and whole-grain bread consumers ( n = 51). The most differential metabolites (variable importance for projection ≥1.5) included compounds originating from cereal plant phytochemicals such as benzoxazinoids and alkylresorcinol metabolites, and compounds produced by gut microbiota (such as enterolactones, hydroxybenzoic and dihydroferulic acid metabolites). Pyrraline, riboflavin, 3-indolecarboxylic acid glucuronide, 2,8-dihydroxyquinoline glucuronide and N-α-acetylcitrulline were also tentatively identified. In order to combine multiple metabolites in a model to predict bread consumption, a stepwise logistic regression analysis was used. Receiver operating curves were constructed to evaluate the global performance of individual metabolites and their combination. The area under the curve values [AUC (95 % CI)] of combined models ranged from 77.8 % (69.1-86.4 %) to 93.7 % (89.4-98.1 %), whereas the AUC for the metabolites included in the models had weak values when they were evaluated individually: from 58.1 % (46.6-69.7 %) to 78.4 % (69.8-87.1 %). Our study showed that a daily bread intake significantly impacted on the urinary metabolome, despite being examined under uncontrolled free-living conditions. We further concluded that a combination of several biomarkers of exposure is better than a single biomarker for the predictive ability of discriminative analysis. [ABSTRACT FROM AUTHOR]

Cucurbitacin C, a bitter substance in Cucumis sativus L., was isolated from green leaves by using phytochemical methods. An analytical method using high-performance liquid chromatography (HPLC) was established for the quantification of cucurbitacin C in different parts of the cucumber plant at different growth periods. Cucurbitacin C was detected in the leaves and stems but not in the female flowers, fruits, roots and leafstalks. The level of cucurbitacin C decreased significantly with the process of young leaves turning old. A new compound named 23,24-dihydrocucurbitacin C, regarded as the next metabolite of cucurbitacin C, was determined unambiguously by HPLC-quadrupole-time-of-flight mass spectrometry and nuclear magnetic resonance. [ABSTRACT FROM AUTHOR]

Metabolic syndrome (MetS) is a serious threat to public health worldwide with an increased risk of developing type 2 diabetes, cardiovascular diseases and all-cause morbidity and mortality. In this study, a urinary metabolomic approach was performed on high performance liquid chromatography quadrupole time-of-flight mass spectrometry to discriminate 36 male MetS patients and 36 sex and age matched healthy controls. Pattern recognition analyses (principal component analysis and orthogonal projections to latent structures discriminate analysis) commonly demonstrated the difference between MetS patients and no-MetS subjects. This study found 8 metabolites that showed significant changes in patients with MetS, including branch-chain and aromatic amino acids (leucine, tyrosine, phenylalanine and tryptophan), short-chain acylcanitine (tiglylcarnitine), tricarboxylic acid (TCA) cycle intermediate (cis-aconitic acid) and glucuronidated products (cortolone-3-glucuronide and tetrahydroaldosterone-3-glucuronide). The candidate biomarkers revealed in this study could be useful in providing clues for further research focusing on the in-depth investigation of the cause of and cure for MetS. [ABSTRACT FROM AUTHOR]

Copyright of Revista de Toxicología is the property of Asociacion Espanola de Toxicologia and its content may not be copied or emailed to multiple sites or posted to a listserv without the copyright holder's express written permission. However, users may print, download, or email articles for individual use. This abstract may be abridged. No warranty is given about the accuracy of the copy. Users should refer to the original published version of the material for the full abstract. (Copyright applies to all Abstracts.)

Hemerocallis citrina Baroni [Asphodelaceae], which is traditional herbal medicine, has been widely used for treating depressive disorders in Eastern-Asia countries. However, the active compounds and corresponding mechanism of anti-depression are not yet completely clarified. In this study, the anti-depressive activities of six H. citrina extracts were primarily evaluated. The results showed that the water extract of H. citrina flowers (HCW) displays significant anti-depressive activity. A total of 32 metabolites were identified from HCW by high-performance liquid chromatography/quadrupole time-of-flight mass spectrometry (HPLC-Q-TOF-MS) and nuclear magnetic resonance (NMR). And then, the anti-depressive activity of the high-level compound (rutin) in HCW was also estimated. The results indicated that rutin displayed significant anti-depressive activity and was one of the main active ingredients. Finally, the anti-depressive mechanisms of HCW and rutin were investigated based on the intestinal microorganisms. The results showed that HCW and rutin increase the diversity and richness of the intestinal flora and regulate the specific intestinal microorganisms such as Bacteroides and Desulfovibrio genera in depressed mice. This work marks the first comprehensive study of the active components, anti-depressive activities and corresponding mechanisms of different H. citrina extracts, which provide a potential possibility for developing new antidepressants., Competing Interests: Author WH was employed by the Green Melody Bioengineering Group Company. The remaining authors declare that the research was conducted in the absence of any commercial or financial relationships that could be construed as a potential conflict of interest., (Copyright © 2022 Liu, Ye, Yang, Zhong, He, Xu, Fang, Deng, Xu, Zeng and Qing.)

Abstract: The approaches for differentiation and dating of gel pen ink entries have been investigated by laser desorption ionization-time of flight mass spectrometry (LDI-TOF-MS) and high performance liquid chromatography-quadruple-time of flight mass spectrometry (HPLC-Q-TOF-MS). 45 kinds of black and blue gel pen ink entries were differentiated individually by the profiles of their LDI-MS spectra. The dye components in the black and blue ink entries have been identified by thin layer chromatography and HPLC-Q-TOF-MS methods. The degradation processes of the dye components in the ink entries under various aging conditions have been probed by LDI-MS approach. The results showed that the variations of relative intensities for the main dye components have a close relationship with aging time, and the degradation of the main dye components were significant under natural storage conditions, which can provide important evidences for dating of the ink entries on paper. [Copyright &y& Elsevier]

Glycerol ester (GE) is a kind of important lipid in milk, which varies greatly depending on many factors. In this study, a novel pseudotargeted lipidomics strategy, named SWATH-MS2&1, was developed for the detection of GEs in milk and the Folch method was selected for the sample preparation. The developed method exhibited a competitive alternative to the acknowledged pseudotargeted strategy, including wider coverage (12 more GEs detected), higher repeatability (12 more GEs, whose coefficient of variation < 0.3), better linearity (5 more GEs, whose R 2 > 0.8), and similar sensitivity (only 2 GEs less than P-MRM after dilution). SWATH-MS2&1 was applied in the investigation of GEs from different milk samples. The orthogonal partial least-squares difference analysis of 219 GEs identified from SWATH-MS2&1 showed satisfying differentiation of different milk samples, and 76 GEs were screened out as potential markers. Our findings demonstrated that SWATH-MS2&1 could offer an accurate method to measure a wide spectrum of GEs in milk.

A sensitive and efficient method was established and validated for qualitative and quantitative analysis of total alkaloids from the extract of Eurycoma longifolia by high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry(HPLC-Q-TOF-MS) combined with ultra-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry(UPLC-QQQ-MS/MS). The HPLC-Q-TOF-MS conditions are as follows: Welch Ultimate XB-C&#95;(18) column(4.6 mm×250 mm, 5 μm) with acetonitrile(containing 0.1% formic acid)-0.1% formic acid in water as mobile phase for gradient elution. The UPLC-QQQ-MS/MS conditions are as below: Agilent Eclipse Plus C&#95;(18) column(2.1 mm×50 mm, 1.8 μm) with acetonitrile(containing 0.1% formic acid) and 0.1% formic acid in water as mobile phase for gradient elution. MS data were collected by electrospray ionization in positive ion mode. According to the comparison with reference standards and the accurate masses of molecules, a total of 17 alkaloids in E. longifolia extract were identified by HPLC-Q-TOF-MS. The UPLC-QQQ-MS/MS quantitative analysis result of 3 alkaloids showed that the linear ranges of them were good(r≥0.999 7) and the overall recoveries ranged from 108.8%-110.2%, with RSDs of 2.9%-5.3%. The method is accurate, reliable, and efficient, which can comprehensively reflect the constituents and content of alkaloids in E. longifolia. The result can serve as a reference for further elucidating its therapeutic material basis and quality control.