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Background/Objectives: The objective of this study was to investigate the metabolomic profiles of patients with colorectal cancer (CRC) across various stages of the disease. Methods: The plasma samples were obtained from 255 subjects, including patients with CRC in stages I-IV, polyps, and controls. We employed capillary electrophoresis time-of-flight mass spectrometry and liquid chromatography triple quadrupole mass spectrometry to analyze hydrophilic metabolites comprehensively. The data were randomly divided into two groups, and consistent differences observed in both groups were analyzed. Results: Acetylated polyamines, such as N1-acetylspermine and N1, N12-diacetylspermine, consistently showed elevated concentrations in stage IV compared to stages I-III. Non-acetylated polyamines, including spermine and spermidine, exhibited increasing trends from polyp to stage IV. Other metabolites, such as histidine and o-acetylcarnitine, showed decreasing trends across stages. While acetylated polyamines have been reported as CRC detection markers, our findings suggest that they also possess diagnostic potential for distinguishing stage IV from other stages. Conclusions: This study showed stage-specific changes in metabolic profiles, including polyamines, of colorectal cancer. [ABSTRACT FROM AUTHOR]

Copyright of Science & Technology of Food Industry is the property of Science & Technology of Food Industry Editorial Office 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.)

Background: Late-onset breast milk jaundice (LBMJ) is a common form of hyperbilirubinemia, which can result in serious complications for newborns with persistently high bilirubin levels. The aim of this study was to investigate the differences in fecal metabolites between breastfed infants with and without LBMJ in order to elucidate potential biological mechanisms. Methods: Biological samples were collected from 12 infants with LBMJ and 12 healthy individuals. Ultra-high performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF/MS) was utilized for non-targeted determination of fecal metabolites. Principal components analysis (PCA), cluster analysis, and differential metabolite analysis were performed in both positive ion mode and negative ion mode for the two groups. Additionally, the KEGG database was employed to comprehensively analyze the pathways of differential metabolites. Results: There were no significant differences in maternal and neonatal demographic characteristics between the two groups (p > 0.05). The results of PCA and cluster heat map analysis in both modes showed that there were significant differences in metabolites between the two groups. Among 751 differential metabolites (DMs) detected in positive ion mode, 720 were up-regulated in the case group while 31 were down-regulated. In negative ion mode, 1891 DMs were detected, including 817 up-regulated metabolites and 1074 down-regulated metabolites in the case group. Analysis of differential metabolic pathways showed that the DMs of the two groups were mainly annotated and enriched in Biotin metabolism, N-Glycan biosynthesis, Taurine and hypotaurine metabolism, Pyrimidine metabolism, and Pentose and glucuronate interconversions. Conclusion: Significant differences exist in fecal metabolites between LBMJ infants and healthy controls. The study of differential metabolic pathways provides insights into the mechanism of LBMJ. [ABSTRACT FROM AUTHOR]

Eupatorium lindleyanum DC. (EL) is a traditional Chinese herb known for its phlegm-reducing, cough-relieving and asthma-calming properties. It is widely used for treating cough and bronchitis. However, preliminary experiments have revealed wide variations in the composition of its different medicinal parts (flowers, leaves and stems), and the composition and efficacy of its different medicinal parts remain largely underexplored at present. In this study, non-targeted rapid resolution liquid chromatography coupled with a quadruple time-of-flight mass spectrometry (RRLC-Q-TOF-MS)-based metabolomics approach was developed to investigate the differences in the chemical composition of different medicinal parts of EL. We identified or tentatively identified 9 alkaloids, 11 flavonoids, 14 sesquiterpene lactones, 3 diterpenoids and 24 phenolic acids. In addition, heatmap visualization, quantitative analysis by high-performance liquid chromatography (HPLC-PDA) and ultra-high-performance liquid chromatography–triple quadrupole tandem mass spectrometry (UPLC-MS/MS) showed particularly high levels of sesquiterpene lactones, flavonoids and phenolic acids in the flowers, such as eupalinolide A and B and chlorogenic acid, among others. The leaves also contained some flavonoid sesquiterpene lactones and phenolic acids, while the stems were almost absent. The findings of in vitro activity studies indicated that the flowers exhibited a notable inhibitory effect on the release of the inflammatory factors TNF-α and IL-6, surpassing the anti-inflammatory efficacy observed in the leaves. Conversely, the stems demonstrated negligible anti-inflammatory activity. The variations in anti-inflammatory activity among the flowers, leaves and stems of EL can primarily be attributed to the presence of flavonoids, phenolic acids and sesquiterpene lactones in both the flowers and leaves. Additionally, the flowers contain a higher concentration of these active components compared to the leaves. These compounds mediate their anti-inflammatory effects through distinct biochemical pathways. The results of this study are anticipated to provide a scientific basis for the rational and effective utilization of EL resources. [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.)

Since the early days of time of flight secondary ion mass spectrometry (ToF-SIMS), increasing the ion signal has been crucial. It is even more crucial when performing tandem mass spectrometry experiments. To achieve this goal, many developments have been made over the years, which are divided into two categories: instrumental development and sample modification. The latter involves sample metallization, matrix deposition, or changing the temperature of the measurement. In this study, the possibility of using matrices to enhance the signals of organic light emitting device (OLED) molecules was explored. Seven molecules commonly used in OLEDs were separately deposited on Si wafers: Alq3, 2,3,5,6-tetrafluoro-7,7,8,8-tetracyanoquinodimethane, 1,4,5,8,9,11-hexaazatriphenylenehexacarbonitrile, Ir(mppy)3, N,N′-bis(naphthalene-1-yl)-N,N′-bis(phenyl)benzidine, 2,2′,7,7′-tetra(N,N-ditolyl)-amino-spiro-bifluor (STTB), and tris(4-carbazoyl-9-ylphenyl)amine. Using the same solvent, three different matrices with different thicknesses, common in matrix assisted light desorption ionization time of flight mass spectrometry, α-cyano-4-hydroxycinnamic acid, 2,5-dihydrobenzoic acid (DHB), and dihydrochloride N-(1-Naphthyl)ethylenediamine, were sprayed on these surfaces. Spectra were acquired for all compounds and spraying conditions in static ToF-SIMS experiments for Alq3 chemical imaging and depth profiling were performed. This allowed the investigation of the fragmentation pattern of the chosen matrices in ToF-SIMS and, thus, obtained a reference for these molecules. The results show that matrices can enhance the signal of fragments of the studied molecules, for example, the signal of STTB is increased with DHB spraying. Samples sprayed only with the solvent were also prepared to verify the impact of the matrices on the signal. Spraying with the solvent alone can enhance the signal even more than the matrices up to four times in the case of Alq3. This result opens new possibilities in the field of matrix-enhanced ToF-SIMS in terms of applications and matrix choices. [ABSTRACT FROM AUTHOR]

Determining water concentrations in the polar regions of the Moon is one of the priority tasks of a number of space missions and, in particular, the Luna-27 mission. The complex of scientific equipment of the Luna-27 spacecraft includes time-of-flight laser ionization mass spectrometer LASMA-LR, the main task of which is to analyze the elemental composition of the regolith at the landing site. The design and configuration of the flight instrument is adapted for the analysis of regolith and was not originally intended for the study of volatile compounds. However, due to the importance of determining the water content in regolith, we reviewed some approaches to analyzing samples during lunar missions and assessed the applicability of LASMA-LR and the laser ionization mass spectrometry method in general for identifying water in regolith. It has been established that using this instrument it is possible to detect water in regolith, including determining its state (chemically bound and unbound water). Moreover, the conditions for sampling the regolith and delivering it to the soil receiving device of the instrument are critically important for the analysis, since under the conditions of the lunar surface, sublimation of ice is possible before the samples are analyzed. This technique has advantages over some other methods of analyzing water and/or ice used in space experiments, and can be used in the study of a number of planets and bodies of the Solar System. [ABSTRACT FROM AUTHOR]

Bletilla striata is the dried tuber of B. striata (Thund.) Reichb.f., which has antibacterial, anti-inflammatory, anti-tumor, antioxidant and wound healing effects. Traditionally, it has been used for hemostasis therapy, as well as to treat sores, swelling and chapped skin. In this study, we used the ultraviolet (UV) absorbance rate of B. striata extracts as the index, and the extraction was varied with respect to the solid–liquid ratio, ethanol concentration, ultrasonic time and temperature in order to optimize the extraction process for its sunscreen components. The main compounds in the sunscreen ingredients of Baiji (B. striata) were analyzed using ultra-high-performance liquid chromatography combined with quadrupole time-of-flight tandem mass spectrometry. The sunscreen properties were subsequently evaluated in vitro using the 3M tape method. The results show that the optimal extraction conditions for the sunscreen components of B. striata were a solid–liquid ratio of 1:40 (g/mL), an ethanol concentration of 50%, an ultrasonic time of 50 min and a temperature of 60 °C. A power of 100 W and an ultrasonic frequency of 40 Hz were used throughout the experiments. Under these optimized conditions, the UV absorption rate of the isolated sunscreen components in the UVB region reached 84.38%, and the RSD was 0.11%. Eighteen compounds were identified, including eleven 2-isobutyl malic acid glucose oxybenzyl esters, four phenanthrenes, two bibenzyl and one α-isobutylmalic acid. An evaluation of the sunscreen properties showed that the average UVB absorption values for the sunscreen samples from different batches of B. striata ranged from 0.727 to 1.201. The sunscreen ingredients of the extracts from B. striata had a good UV absorption capacity in the UVB area, and they were effective in their sunscreen effects under medium-intensity sunlight. Therefore, this study will be an experimental reference for the extraction of sunscreen ingredients from the B. striata plant, and it provides evidence for the future development of B. striata as a candidate cosmetic raw material with UVB protection properties. [ABSTRACT FROM AUTHOR]

Context: Qi‐dan‐dihuang decoction (QDD) has been used to treat diabetic kidney disease (DKD), but the underlying mechanisms are poorly understood. Objective: This study reveals the mechanism by which QDD ameliorates DKD. Materials and Methods: The compounds in QDD were identified by high‐performance liquid chromatography and quadrupole‐time‐of‐flight tandem mass spectrometry (HPLC‐Q‐TOF‐MS). Key targets and signaling pathways were screened through bioinformatics. Nondiabetic Lepr db/m mice were used as control group, while Lepr db/db mice were divided into model group, dapagliflozin group, 1% QDD‐low (QDD‐L), and 2% QDD‐high (QDD‐H) group. After 12 weeks of administration, 24 h urinary protein, serum creatinine, and blood urea nitrogen levels were detected. Kidney tissues damage and fibrosis were evaluated by pathological staining. In addition, 30 mmol/L glucose‐treated HK‐2 and NRK‐52E cells to induce DKD model. Cell activity and migration capacity as well as protein expression levels were evaluated. Results: A total of 46 key target genes were identified. Functional enrichment analyses showed that key target genes were significantly enriched in the phosphatidylinositol 3‐kinase (PI3K)/protein kinase B (AKT) and mitogen‐activated protein kinase (MAPK) signaling pathways. In addition, in vivo and in vitro experiments confirmed that QDD ameliorated renal fibrosis in diabetic mice by resolving inflammation and inhibiting the epithelial‐mesenchymal transition (EMT) via the p38MAPK and AKT‐mammalian target of rapamycin (mTOR) pathways. Discussion and Conclusion: QDD inhibits EMT and the inflammatory response through the p38MAPK and AKT/mTOR signaling pathways, thereby playing a protective role in renal fibrosis in DKD. [ABSTRACT FROM AUTHOR]

Newborn screening (NBS) for sickle cell disease (SCD) requires a robust, high-throughput method to detect hemoglobin S (HbS). Screening for SCD is performed by qualitative methods, such as isoelectric focusing (IEF), and both qualitative and quantitative methods such as high performance liquid chromatography (HPLC), capillary electrophoresis (CE), and tandem mass spectrometry (MS/MS). All these methods detect HbS, as well as low-level or absent HbA, and also other variants of hemoglobin. HPLC is considered as a reference method for NBS, because of its high sensitivity and specificity in detecting HbS. NeoSickle®, a fully automated matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS) platform, combined with automated sample processing, a laboratory information management system and NeoSickle® software for automatic data interpretation, has increased the throughput of SCD testing. The purpose of this study was to compare the performances of NeoSickle® and HPLC. A prospective study was conducted including 9,571 samples from the NBS program to compare MALDI-MS using NeoSickle® with an HPLC method. Correlation between the two methods was studied. For the MALDI-MS method, sensitivity, specificity, NPV, and PPV were calculated. We found over 99.4 % correlation between the HPLC and MALDI-MS results. NeoSickle® showed 100 % of sensitivity and specificity in detecting SCD syndrome, leading to positive and negative predictive values of 100 %. NeoSickle® is adapted to NBS for SCD, and can be used in first-line high-throughput screening to detect HbS, and beta-thalassemia major warning. When HbS is detected, second-line use of another specific method as HPLC is necessary. [ABSTRACT FROM AUTHOR]

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

Objective The rhizome of Atractylodes macrocephala Koidz. (Asteraceae), called Atractylodes macrocephala rhizome (AMR) and known by its traditional name Bai Zhu, is a prominent Chinese herbal medicine employed for preventing miscarriage. However, our previous study revealed that high dosages of AMR administered during pregnancy could cause embryotoxicity but the specific embryotoxic components and their underlying mechanisms remain unclear. This study aimed to screen and identify the potential embryotoxic components of AMR. Methods The AMR extracts and sub-fractions were analyzed by thin layer chromatography and subsequently screened by in vitro mouse limb bud micromass and mouse whole embryo culture bioassays. The embryotoxic fractions from AMR were further evaluated in vivo using a pregnant mouse model. The structures of the potential embryotoxic components were analyzed using matrix-assisted laser desorption/ionization tandem time-of-flight mass spectrometry (MALDI-TOF/TOF-MS). Results In vitro and in vivo bioassays revealed that AMR glycoside-enriched sub-fractions (AMR-A-IIa and AMR-A-IIb) exhibited potential embryotoxicity. These sub-fractions, when administered to pregnant animals, increased the incidence of stillbirth and congenital limb malformations. MS spectrometry analysis identified cycasin derivatives in both sub-fractions, suggesting their possible role in the observed limb malformations. However, further experiments are necessary to validate this hypothesis and to elucidate the underlying mechanisms. Conclusions Our study provides significant scientific evidence on the pharmacotoxicity of AMR, which is important for the safe clinical application of commonly used Chinese herbal medicines during pregnancy. [ABSTRACT FROM AUTHOR]

Phytophthora parasitica is an oomycete pathogen that infects a broad range of crops of worldwide economic interest; among them are citrus species. In general, some Citrus and the rootstocks of related genera offer considerable resistance against P. parasitica; therefore, understanding the mechanisms involved in the virulence of this pathogen is crucial. In this work, P. parasitica secondary metabolite production was studied using matrix-assisted laser desorption/ionization mass spectrometry imaging (MALDI-MSI) and ultrahigh-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UHPLC/ESI-Q-TOF-MS) combined with chemometric tools, and its metabolic profile was evaluated under the influence of Citrus sunki (a highly susceptible host) and Poncirus trifoliata (a resistant genotype) extracts. The root extracts of Citrus sunki had an influence on the growth and hyphae morphology, and the root extracts of P. trifoliata had an influence on the zoospore behavior. In parallel, the spatial distribution of several metabolites was revealed in P. parasitica colonies using MALDI-MSI, and the metabolite ion of m/z 246 was identified as the protonated molecule of Arg-Ala. The MALDI-MSI showed variations in the surface metabolite profile of P. parasitica under the influence of the P. trifoliata extract. The P. parasitica metabolome analysis using UHPLC-ESI-Q-TOF-MS resulted in the detection of Arg-Gln (m/z 303.1775), as well as L-arginine (m/z 175.1191) and other unidentified metabolites. Significant variations in this metabolome were detected under the influence of the plant extracts when evaluated using UHPLC-ESI-Q-TOF-MS. Both techniques proved to be complementary, offering valuable insights at the molecular level when used to assess the impact of the plant extracts on microbial physiology in vitro. The metabolites identified in this study may play significant roles in the interaction or virulence of P. parasitica, but their functional characterization remains to be analyzed. Overall, these data confirm our initial hypotheses, demonstrating that P. parasitica has the capabilities of (i) recognizing host signals and altering its reproductive programing and (ii) distinguishing between hosts with varying responses in terms of reproduction and the production of secondary metabolites. [ABSTRACT FROM AUTHOR]

Background: Trapa bispinosa shells (TBs) and its flesh (TBf) have been recognized for their medicinal properties, including antioxidant, antitumor, and immunomodulatory effects. Despite these benefits, TBs are often discarded as waste material, and their applications remain to be further explored. Methods: In this study, we optimized the solid-state fermentation process of Ganoderma sinense (GS) with TBs using a response surface experiment methodology to obtain the fermented production with the highest water extract rate and DPPH free radical scavenging activity. We prepared and characterized pre-fermentation purified polysaccharides (P1) and post-fermentation purified polysaccharides (P2). Alcoholic extracts before (AE1) and after (AE2) fermentation were analyzed for active components such as polyphenols and flavonoids using UPLC-QTOF-MS/MS (ultra-performance liquid chromatography–quadrupole time-of-flight tandem mass spectrometry). Mouse macrophages (RAW 264.7) were employed to compare the immune-stimulating ability of polysaccharides and the antioxidant activity of AE1 and AE2. Results: Optimal fermentation conditions comprised a duration of 2 days, a temperature of 14 °C, and a humidity of 77%. The peak water extract yield and DPPH free radical scavenging rate of the water extract from TBs fermented by GS were observed under these conditions. The enhanced activity may be attributed to changes in the polysaccharide structure and the components of the alcoholic extract. The P2 treatment group indicated more secretion of RAW 264.7 cells of NO, iNOS, IL-2, IL-10, and TNF-α than P1, which shows that the polysaccharides demonstrated increased immune-stimulating ability, with their effect linked to the NF-кB pathway. Moreover, the results of the AE2 treatment group indicated that secretion of RAW 264.7 cells of T-AOC and T-SOD increased and MDA decreased, which shows that the alcoholic extract demonstrated enhanced antioxidant activity, with its effect linked to the Nrf2/Keap1-ARE pathway. Conclusions: Biphasic fermentation of Trapa bispinosa shells by Ganoderma sinense could change the composition and structure of the polysaccharides and the composition of the alcoholic extract, which could increase the products' immunomodulatory and antioxidant activity. [ABSTRACT FROM AUTHOR]

Ulcerative colitis (UC) is an inflammatory disease with abdominal pain, diarrhea, and bloody stool as the main symptoms. Several studies have confirmed that polysaccharides are effective against UC. It is commonly accepted that the traditional benefits of Radix Codonopsis can be attributed to its polysaccharide contents, and inulin-type fructan CP-A is the main active monomer in the polysaccharide components. Herein, we established a 2,4,6-trinitrobenzene sulfonic acid (TNBS)-induced UC rat model and lipopolysaccharide (LPS)-induced colonic epithelial cell model (NCM460) to investigate the effect of CP-A on UC. Untargeted metabolomics studies were conducted to identify differential metabolites using ultra-high performance liquid chromatography quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF/MS) and enrich metabolic pathways in rat serum. The in vivo assays demonstrated that CP-A reduces colonic macroscopic injury, disease activity index (DAI), histopathological score, interleukin (IL)-8, and tumor necrosis factor-a (TNF-a) levels, as well as the expression of intercellular adhesion molecules. On the other hand, CP-A increases IL-10 and transforming growth factor-b (TGF-b) levels. The in vitro experiments indicated that CP-A treatment could reduce nitric oxide (NO) and IL-1b after LPS stimulation. The metabolomics results suggested that CP-A therapy for UC may be related to the mammalian target of rapamycin (mTOR) signaling pathway. The in vitro and in vivo validation of the pathway showed similar results, indicating that CP-A alleviates UC by preventing the activation of mTOR/p70S6K signaling pathway. These findings offer a fresh approach to treating UC and a theoretical foundation for the future advancement of CP-A. [ABSTRACT FROM AUTHOR]

FLH 13-11 is an F1 interspecific hybrid muscadine grape genotype that was developed to produce new anthocyanins for pigment color stability. This hybrid resulted from a cross between 'Marsh' (Vitis munsoniana) and 'Magoon' (V. rotundifolia) and has been cultivated for the wine and juice industry. This report characterizes anthocyanins produced in fully ripe berries and reveals a significant difference in total anthocyanin contents from two continuous cropping seasons. High-performance liquid chromatography with a diode array detector (HPLC-DAD) and HPLC–quadrupole time-of-flight tandem mass spectrometry (HPLC-qTOF-MS/MS) were used to profile anthocyanins in berries. The resulting data showed that fourteen anthocyanins were detected, six from 2011 and nine from 2012, with only one produced in both seasons. However, the anthocyanidin profiles of the berries were the same. Five anthocyanins were annotated as diglucosides of anthocyanidins based on MS/MS features, including delphinidin 3,5-diglucoside produced in both seasons, cyanidin 3,5-diglucoside mainly formed in 2011, petunidin 3,5-diglucoside, malvidin 3,5-diglucoside, and peonidin 3,5-glucoside only detected in 2012. Also, three anthocyanidin-diglucoside-like anthocyanins and three monoglucosides, including peonidin 3-glucoside, delphinidin 3-glucoside like, and pelargonidin 3-glucoside-like anthocyanins, were detected in 2011 and 2012, respectively. These results indicate that FLH 13-11 can produce both anthocyanidin-diglucosides and -monoglucosides, and their biosynthesis is closely dependent on cropping years. [ABSTRACT FROM AUTHOR]

Capsaicinoids are the main bioactive compounds in hot chili peppers. In the present work, Ultra-performance liquid chromatography coupled with a photodiode detector-quadrupole and tandem time-of-flight mass spectrometry detector (UPLC-ESI-Q-TOF-MS/PDA) was established to characterize, identify and quantify 7 capsaicinoid derivatives based on their MS spectra, and comparisons with standards when available, as well as with literature data. According to the systematic analysis of the collected MS spectra and the observed fragmentation, the detected compounds were glycosylated and acylated capsaicinoids. Namely, capsaicin-glucoside, dihydrocapsaicin-glucoside, nordihydrocapsaicin-glucoside, homocapsaicin-glucoside and homodihydrocapsaicin-glucoside, beside capsaicin-ferulate and dihydrocapsaicin-ferulate, were isolated for the first time from pepper cultivars. Capsaicinoid-glucoside were detected in Xingshuzaohui and Shuailiang cultivars (cultivated in a greenhouse), while capsaicinoid-ferulate were detected in Hangzhou and Xiaomila cultivars. The capsaicinoid-glucoside content ranged from 6.93 to 9.85 mg/kg of fresh weight, while total capsaicinoid-ferulate content ranged from 1.79 to 3.78 mg/kg. The changes in the content of the detected capsaicinoid derivatives depended on the pepper-cultivated method and maturity stages. The scatterplot demonstrated a strong correlation between pepper extracts' anti-oxidant activity (DPPH and ABTS) and their capsaicinoid content, particularly capsaicin-glucoside. [ABSTRACT FROM AUTHOR]

Phellodendri Amurensis Cortex (PAC) is a medicinal herb that has been generally used to treat diarrhea and jaundice. In order to comprehensively evaluate the PAC in the main production areas quality, a qualitative and quantitative method with highly effective, sensitive, and reliable was developed. The chemical compositions of PAC were analyzed, and fingerprints were established by ultra‐high‐performance liquid chromatography‐quadrupole time‐of‐flight tandem mass spectrometry (UPLC‐Q‐TOF‐MS). Then, the determination of berberine, canthin‐6‐one, dictamnine, γ‐fagarine, and magnoflorine from PAC samples was simultaneously performed using UPLC‐QQQ‐MS. Furthermore, the chemical components of PAC from different regions were compared and analyzed by combining hierarchical cluster analysis, principal component analysis, and orthogonal partial least squares discriminant analysis. A total of 58 compounds were identified, including 36 alkaloids, four phenylpropanoids, seven terpenoids, four flavonoids and their glycosides, an organic acid compound, and six other components. The fingerprint results show that samples have good similarity. Meanwhile, the content of the five ingredients in different habitats is quite different. By multivariate statistical analysis, 18 batches of PAC could be divided into three categories, and 20 components were identified as differential markers of various origins. A comprehensive method of PAC quality evaluation and chemical composition difference analysis was established, which provided the scientific basis for quality evaluation and further pharmacological mechanism research. [ABSTRACT FROM AUTHOR]

Background: The Jiawei Kongsheng Zhenzhong pill (JKZP), a Chinese herbal prescription comprised of eight Chinese crude drugs, has been historically employed to treat neurological and psychological disorders. Nevertheless, the ambiguous material basis severely hindered its progress and application. Purpose: The current study aimed to establish a rapid analytical method for identifying the chemical components of the JKZP aqueous extract and the components absorbed into the rat serum to investigate the quality markers (Q-markers) responsible for the neuroprotective effects of JKZP. Methods: The qualitative detection of the chemical components, prototype components, and metabolites of the aqueous extracts of JKZP, as well as the serum samples of rats that were administered the drug, was performed using the ultra-performance liquid chromatography- quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS) technology. This analysis combined information from literature reports and database comparisons. Moreover, the study was conducted to anticipate the potential Q-markers for the neuroprotective effects of JKZP based on the "five principles" of Q-marker determination. Results: A total of 67 compounds and 111 serum components (comprising 33 prototypes and 78 metabolites) were detected and identified. Combining the principles of quality transmission and traceability, compound compatibility environment, component specificity, effectiveness, and measurability, the study predicted that five key compounds, namely, senkyunolide H, danshensu, echinacoside, loganin, and 3,6'-disinapoyl sucrose, may serve as potential pharmacological bases for the neuroprotective effects of JKZP. Conclusion: To summarize, the UPLC-Q-TOF-MS/MS technique can be employed to rapidly and accurately identify compounds in JKZP. Five active compounds have been predicted to be the Q-markers for the neuroprotective effects of JKZP. This discovery serves as a reference for improving quality, advancing further research and development, and utilizing Chinese herbal prescriptions. [ABSTRACT FROM AUTHOR]

Introduction: Roses are one of the most essential ornamental flowers and are commonly used in perfumery, cosmetics, and food. They are rich in bioactive compounds, which are of interest for therapeutic effects. Objectives: The objective of this study was to understand the kinds of changes that occur between the nocturnal and diurnal metabolism of rose and to suggest hypotheses. Methods: Reversed-phase ultrahigh-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry or triple quadrupole mass spectrometry (TQ MS/MS) was used for nontargeted metabolomics and hormonal profiling respectively. For metabolite annotation, accurate mass spectra were compared with those in databases. Results: The hormonal profile of flowers showed an increase in jasmonate at night, while that of leaves indicated an increase in the salicylic acid pathway. Nontargeted analyses of the flower revealed a switch in the plant's defense mechanisms from glycosylated metabolites during the day to acid metabolites at night. In leaves, a significant decrease in flavonoids was observed at night in favor of acid metabolism to maintain a level of protection. Moreover, it might be possible to place back some of the annotated molecules on the shikimate pathway. Conclusion: The influence of day and night on the metabolome of rose flowers and leaves has been clearly demonstrated. The hormonal modulations occurring during the night and at day are consistent with the plant circadian cycle. A proposed management of the sesquiterpenoid and triterpenoid biosynthetic pathway may explain these changes in the flower. In leaves, the metabolic differences may reflect night-time regulation in favor of the salicylic acid pathway. [ABSTRACT FROM AUTHOR]

Rationale: Pyrrolidone‐based drugs find widespread use in treating conditions such as epilepsy and Alzheimer's disease, and in various other medical applications. Brivaracetam, the latest generation of pyrrolidone drugs, has exhibited significant promise owing to chemical structure modifications. Its affinity to the SV2A receptor is double that of the previous‐generation drug, levetiracetam. Consequently, brivaracetam holds substantial potential for diverse applications. As a novel drug not yet included in the pharmacopeias of developed nations, comprehensive analysis and research are necessary to guarantee its safe utilization in clinical settings. Methods: A liquid chromatography quadrupole time‐of‐flight tandem mass spectrometry (LC/QTOFMS) method has been developed to effectively separate, identify and characterize both the degradation products and process‐related substances of brivaracetam. Stress testing of the sample was carried out following the guidelines outlined in ICH Q1A(R2). The structures of these impurities were identified through positive electrospray ionization QTOF high‐resolution MS and NMR spectroscopy. Additionally, the formation mechanism of each degradation product is thoroughly discussed. Results: Under the analytical conditions outlined in this paper, brivaracetam and its degradation products were effectively separated. Thirteen degradation products were detected and characterized, shedding light on their origins and degradation pathways. Among these, three degradation products align with previously reported impurities, and two unreported degradation products were synthesized and confirmed through NMR spectroscopy. The stress testing results revealed the instability of brivaracetam under acidic, alkaline, oxidative and thermal stress conditions, while it exhibited relative stability under photolytic stress conditions. Conclusion: The study developed an analytical method for brivaracetam that enabled the effective detection and separation of brivaracetam and its 13 degradation products. This method addresses a gap in both current domestic and foreign drug standards. The structures of all the major degradation products were characterized by high‐resolution LC/QTOFMS, which is essential for quality control during the drug production process, stability evaluation and the establishment of proper storage conditions. [ABSTRACT FROM AUTHOR]

Fufang Xiling Jiedu capsule (FXJC), a traditional Chinese medicine that evolved from "Yinqiao Powder", is widely used for the treatment of cold and influenza. However, due to a lack of in vivo metabolism research, the chemical components responsible for the therapeutic effects still remain unclear. Hence, this study aimed to describe the metabolic profiles of the FXJC in rat plasma, urine, and feces. A combined data mining strategy based on ultra‐performance liquid chromatography coupled with quadrupole time‐of‐flight tandem mass spectrometry was employed and 201 xenobiotics, including 117 prototype components and 84 metabolites were detected. Phenolic acids, flavonoids, triterpenes, and lignans were prominent ingredients absorbed in vivo, and the major metabolic pathways of the detected metabolites were glucuronidation, sulfation, methylation, and oxidation. This is the first systematic study on the metabolism of the FXJC in vivo, providing valuable information for future studies on the efficacy, toxicity, and mechanism of the FXJC. [ABSTRACT FROM AUTHOR]

Qiangli Dingxuan (QLDX) tablet is a widely recognized traditional Chinese medicine formula that has been extensively used in China for decades to treat vertigo, tinnitus, and dizziness owing to its outstanding therapeutic outcomes. However, the complexity of the chemical components in this tablet makes it challenging to separate and identify these components. This study presented an effective and sensitive strategy for the rapid separation and simultaneous structural identification of QLDX tablet components using ultra‐performance liquid chromatography with quadrupole time‐of‐flight tandem mass spectrometry and the UNIFI platform. Based on retention times, accurate masses, fragment ions, related literature, and authentic standards, 119 compounds were identified or tentatively characterized; these included 9 iridoids, 12 lignans, 21 phenylpropanoids, 27 flavonoids, 7 phthalides, and 43 others. Among them, 36 were confirmed using reference standards. The representative compounds with various chemical structures were studied by analyzing their fragmentation patterns and characteristic ions. In conclusion, this study established a rapid approach for characterizing the chemical constituents in QLDX tablet. The proposed approach provides a basis for qualitative analysis and quality control in the manufacturing process and is beneficial for advancing investigations into the efficacy and mechanism of action of this tablet. [ABSTRACT FROM AUTHOR]

Dietary supplements used for improving brain function and strengthening attention are increasingly popular. However, illegal dietary supplements containing unapproved drugs continue to be seized. Therefore, it is necessary to rapidly screen and identify adulterated compounds in dietary supplements for public safety. To develop the simultaneous analytical method, we selected 11 nootropic compounds and optimized the simultaneous liquid chromatography‐electrospray ionization‐tandem mass spectrometry and optimal conditions for liquid chromatography‐quadrupole time‐of‐flight mass spectrometry were proposed to determine the fragmentation patterns of each compound. The specificity, linearity, limit of detection, limit of quantification, method detection limit, method quantitation limit, precision, accuracy, matrix effect, and stability of this method were evaluated according to international validation guidelines. The validated methods were applied to 54 samples containing dietary supplements and seized samples. On screening 11 nootropic compounds were detected in four solid samples (tablet and powder). By comparing the product ion ratios with the standards and quantification, vinpocetine (6.52–34.2 mg/g) was found in three samples, and omberacetam (995.6 mg/g) in one sample. To re‐confirm the detected compounds, the fragmentation patterns were compared with those of the standards using liquid chromatography‐quadrupole time‐of‐flight mass spectrometry. The developed simultaneous analysis method can help maintain public health and safety. [ABSTRACT FROM AUTHOR]

Illegal drugs are becoming a public health problem in African cities. In 2021, Bombé, a new drug of unknown composition, caused an outbreak of neuro-psychiatric symptoms in Kinshasa. Bombé was rumored to be based on ground catalytic exhausts stolen from cars. The chemical composition of six samples of Bombé obtained from different neighborhoods in Kinshasa was determined by triple quad liquid chromatography-mass spectrometry/mass spectrometry with confirmation by quadrupole time-of-flight mass spectrometry. Metals were determined by inductively coupled plasma-mass spectrometry, and polycyclic aromatic hydrocarbons were measured by gas chromatography-mass spectrometry. Analysis of the Bombé samples revealed that it contained heroin (2–12% of the total area under the curve of the samples) and opioid derivatives, plus paracetamol (33–72%), caffeine (17–26%), and also benzodiazepines (5/6 samples) and cyproheptadine (2/6 samples). The concentrations of neurotoxic metals were unremarkable. The median (range) concentrations of manganese and lead were 9.4 µg/g (range 3–334 μg/g) and 0.36 µg/g (range 0.1–3.12 μg/g), respectively. All polycyclic aromatic hydrocarbons were below the level of detection (<0.10 µg/g). Thanks to international collaboration, Bombé was documented to be a heroin-based drug and its alleged origin from catalytic exhausts was not substantiated. The local human expertise and technical capacity for undertaking toxicological analyses should be increased in Africa. [ABSTRACT FROM AUTHOR]

Physochlainae Radix (PR) is an essential herbal medicine that has been generally applied for treating cough and asthma. In this study, a comprehensive strategy for quality evaluation of PR from different origins was established by integrating qualitative identification, quantitative analysis, and chemometric methods. A total of 58 chemical components were identified by ultra‐high‐performance liquid chromatography coupled with quadrupole time‐of‐flight tandem mass spectrometry (UHPLC‐Q‐TOF‐MS/MS), and a sensitive and rapid UHPLC‐QqQ‐MS/MS method was established for the simultaneous determination of 12 compounds. In addition, multivariate statistical analysis was applied for discriminant analysis to compare the differences among 30 batches of PR samples. The results showed that the 30 batches of PR collected from four provinces could be clustered into three categories, in which scoparone, protocatechuic acid, tropic acid, and scopolin were important components to distinguish the primary and non‐primary producing areas, as well as superior and inferior products of PR. Chemometric results were consistent and validated each other, and systematically explained the intrinsic quality characteristics of PR. This study first demonstrated that LC‐MS combined with multivariate statistical analysis, provided a comprehensive and effective means for quality evaluation of PR. [ABSTRACT FROM AUTHOR]

Background: Xiao-Er-An-Shen decoction (XEASD), a TCM formula composed of sixteen Chinese medicinal herbs, has been used to alleviate tic disorders (TD) in clinical practice for many years. However, the chemical basis underlying the therapeutic effects of XEASD in the treatment of TD remains unknown. Purpose: The present study aimed to determine the major chemical components of XEASD and its prototype compounds and metabolites in mice biological samples. Methods: The chemical constituents in XEASD were identified using ultra-high Performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS). Following this, XEASD was orally administered to mice, and samples of plasma, urine, feces, bile, and tissue were collected in order to identify effective compounds for the prevention or treatment of TD. Result: Of the total 184 compounds identified to be discriminated in the XEASD, comprising 44 flavonoids, 26 phenylpropanoids, 16 coumarins, 16 triterpenoids, 14 amino acids, 13 organic acids, 13 alkaloids, 13 ketones, 10 cyclic enol ether terpenes, 7 citrullines, 3 steroids, and 5 anthraquinones, and others. Furthermore, we summarized 54 prototype components and 78 metabolic products of XEASD, measured with biological samples, by estimating metabolic principal components, with four prototype compounds detected in plasma, 58 prototypes discriminated in urine, and 40 prototypes identified in feces. These results indicate that the Oroxylin A glucuronide from Citri reticulatae pericarpium (CRP) is a major compound with potential therapeutic effects identified in brain, while operating positive effect in inhibiting oxidative stress in vitro. Conclusion: In summary, our work delineates the chemical basis underlying the complexity of XEASD, providing insights into the therapeutic and metabolic pathways for TD. Various types of chemicals were explored in XEASD, including flavonoids, phenylpropanoids, coumarins, organic acids, triterpenoid saponins, and so on. This study can promote the further pharmacokinetic and pharmacological evaluation of XEASD. [ABSTRACT FROM AUTHOR]

Introduction: Twisted-leaf garlic (Allium obliquum L.) is a wild Allium species, which is traditionally used as aroma plant for culinary purposes due to its unique, garlic-like flavor. It represents an interesting candidate for domestication, breeding and cultivation. Objectives: The objective of this work was to explore and comprehensively characterize polar and semi-polar phytochemicals accumulating in leaves and bulbs of A. obliquum. Method: Plant material obtained from a multiyear field trial was analyzed using a metabolite profiling workflow based on ultra-high performance liquid chromatography-coupled electrospray ionization quadrupole time-of-flight mass spectrometry (UHPLC/ESI-QTOFMS) and two chromatographic methods. For annotation of metabolites, tandem mass spectrometry experiments were carried out and the resulting accurate-mass collision-induced dissociation (CID) mass spectra interpreted. Onion and garlic bulb extracts were used as reference samples. Results: Important metabolite classes influencing nutritional, sensory and technological properties were detected and structurally characterized including fructooligosaccharides with a degree of polymerization of 3–5, S-alk(en)ylcysteine sulfoxides and other S-substituted cysteine conjugates, flavonoids including O- and C-glycosylated flavones as well as O-glycosylated flavonols, steroidal saponins, hydroxycinnamic acid conjugates, phenylethanoids and free sphingoid bases. In addition, quantitative data for non-structural carbohydrates, S-alk(en)ylcysteine sulfoxides and flavonoids are provided. Conclusion: The compiled analytical data including CID mass spectra of more than 160 annotated metabolites provide for the first time a phytochemical inventory of A. obliquum and lay the foundation for its further use as aroma plant in food industry. [ABSTRACT FROM AUTHOR]

We report a collision‐induced dissociation (CID) based gas phase rearrangement study using quadrupole time‐of‐flight mass spectrometry coupled with liquid chromatography on a novel endothelin and angiotensin II receptor antagonist, sparsentan. We performed tandem mass spectrometry to identify precursor and fragment ion relationships and assigned structures for major fragment ions. We propose a benzyl migration mechanism based on bond length measurements in density functional theory (B3LYP/6‐31+G*) optimized geometries of protonated sparsentan and its m/z 547 fragment. Protonated sparsentan undergoes loss of ethanol, which yields a resonance‐stabilized benzylic cation with m/z 547, which further fragments into m/z 353 via benzyl migration, where the benzylic cation migrates to one of the nucleophilic nitrogen atoms followed by proton transfer from the sulfonamide nitrogen to a carbonyl oxygen, resulting in a neutral loss of mass 194. Further fragmentation of m/z 353 results in m/z 258, which undergoes radical and neutral loss to yield m/z 193 and 194, respectively. The proposed mechanism of generation of m/z 353 was confirmed by CID of deuterated sparsentan. Considering the importance of gas phase rearrangements of organic molecules in structural identifications as well as the novelty of the molecule, these findings will be helpful for future studies to predict gas phase benzyl migration in sparsentan analogs and for degradation product and metabolite identification of sparsentan and its analogs using LC–MS. [ABSTRACT FROM AUTHOR]

Edible bird's nest (EBN) is a valuable and nutritious food tonic made from the saliva of swiftlet birds. EBN has been consumed for centuries due to its high nutritional value. Proteins are the main nutrient in EBN. However, studies investigating the functional proteins in EBN are still limited. Therefore, the present study aims to characterize the functional proteins from EBN using proteomic-based techniques. In addition, the molecular characteristics of the functional proteins were analyzed using sodium dodecyl sulfate–polyacrylamide gel electrophoresis (SDS-PAGE). The results showed that 0.951 ± 0.03 mg/mL of functional proteins were successfully extracted from the EBN. Several distinct protein bands in the range of 35–135 kDa were profiled from the EBN. Using ultrahigh-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF-MS-MS), a total of 51 proteins were identified from the EBN. The protein sequences were processed in the BIOPEP database to predict the potential biological activity of EBN proteins. The prediction results suggest that EBN proteins potentially possess antioxidant, anti-inflammatory, immunostimulatory, antiamnestic, antihypertensive (angiotensin-converting enzyme (ACE) inhibitors), antidiabetic (alpha-glucosidase inhibitors, alpha-amylase inhibitors, dipeptidyl peptidase IV inhibitors), and antithrombotic properties. The antioxidant properties (DPPH-scavenging activity (20.84% ± 3.43) and ABTS-scavenging activity (31.49% ± 1.66)) and anti-inflammatory properties (inhibition of nitric oxide (NO) production (21.30% ± 4.41) and inhibition of albumin denaturation (25.30% ± 0.32)) were experimentally validated. In conclusion, the results suggest that functional proteins from EBN are potentially functional ingredients in the nutraceutical and food industries. [ABSTRACT FROM AUTHOR]

The herb Fissistigma oldhamii var. longistipitatum has been used for a long time in Asian folk medicine in the treatment of several diseases, including rheumatoid arthritis and other inflammatory conditions. Researchers in China and elsewhere have analyzed and characterized its chemical content. In this study, a UHPLC-Q-TOF-MS/MS method, run in both positive and negative modes, was used to identify the main chemical compounds in dichloromethane extracts of this F. oldhamii variant. A total of 64 compounds, including 44 alkaloids and 20 flavonoids, were rapidly identified or tentatively characterized by comparing the molecular ion peaks and MS2 mass spectrometry fragment ions, combined with the mass spectrometry information of reference substances, appropriate fragmentation ions and related literatures. For the first time, the developed UHPLC-Q-TOF-MS/MS analysis method allows for the determination of 64 compounds from extracts of the F. oldhamii variant. The method presented here produced results that will be useful in further studies of this herb. [ABSTRACT FROM AUTHOR]

Objectives: To evaluate the ability of the aqueous extract of Mitracarpus frigidus (MFAq) to inhibit lipid body formation and inflammatory mediator production in macrophages stimulated with lipopolysaccharide (LPS) and interferon gamma (IFN-γ). Methods: MFAq was chemically characterized by ultrafast liquid chromatography/quadruple time-of-flight tandem mass spectrometry. The macrophages obtained from mice were incubated with MFAq. Cell viability and membrane integrity were evaluated by 3-(4,5-dimethylthiazol-2-yl)-2,5-diphenyltetrazolium bromide and propidium iodide assays, respectively. Moreover, NO, reactive oxygen species (ROS), transforming growth factor beta (TGF-β), prostaglandin E2 (PGE2) levels and lipid bodies (LBs) were examined in macrophages that were stimulated with LPS and IFN-γ and treated with MFAq. Finally, molecular docking analysis was conducted to investigate the interaction of MFAq with the cyclooxygenase 2 (COX-2) enzyme. Key findings: Chlorogenic acid, clarinoside, harounoside, rutin, kaempferol-3O-rutinoside and 2-azaanthraquinone were identified in MFAq. MFAq significantly inhibited NO, ROS and LBs, and did not affect the membrane integrity of macrophages. MFAq-treated cells showed significantly lower levels of TGF-β and PGE2. Molecular docking demonstrated that the compounds found in MFAq are able to inhibit COX-2 by binding to important residues in the catalytic site. Conclusions: MFAq interferes with lipid metabolism in stimulated macrophages, leading to the reduction of important inflammatory mediators. Furthermore, MFAq can directly inhibit the COX-2 enzyme or inhibit its expression owing to its ability to reduce NO production. [ABSTRACT FROM AUTHOR]

Rationale: The flower of Citrus aurantium L. var. amara Engl. (FCAVA), an edible tea and herbal medicine with anti‐obesity effect, has attracted great attention in China. The structural elucidation of chemical components in FCAVA has been realized in our previous work. It is well known that metabolic profiling provided a structural basis to discover potential anti‐obesity ingredients in FCAVA. Nevertheless, there are no reports about in vivo metabolic profiles of FCAVA. Therefore, it is necessary to comprehensively identify in vivo substances of FCAVA. Methods: The identification of in vivo substances of FCAVA remains a challenge due to the strong interference of complex chemical components, biological matrices and metabolite isomers. In this work, ultra‐high‐performance liquid chromatography coupled to quadrupole time‐of‐flight tandem mass spectrometry (UHPLC‐QTOF‐MS/MS) analysis with a data mining strategy was established and applied for the metabolic profiling of FCAVA in rats. The data mining strategy, including diagnostic product ions and neutral loss filtering, improved structural elucidation of xenobiotics in rats after oral administration of FCAVA. Results: A total of 228 xenobiotics, including 80 prototypes (10 unambiguous confirmed with reference standards) and 148 metabolites, were tentatively characterized in rat plasma, urine and fecal samples. Among them, 35 xenobiotics were found in plasma, 124 in urine and 156 in feces. The main biotransformation pathway of FCAVA metabolism was deglycosylation, methylation, glucuronidation and sulfation. The main compounds absorbed into the blood were neohesperidin and naringin, which have been reported to show significant anti‐obesity effect. Conclusions: Collectively, this present study would be conducive to the discovery of active ingredients of FCAVA for the treatment of obesity and the development of quality control of FCAVA. [ABSTRACT FROM AUTHOR]

This work describes a comprehensive achiral × chiral two‐dimensional liquid chromatography separation for enantioselective amino acid analysis coupled to electrospray ionization‐tandem mass spectrometry detection using data‐independent acquisition. Flow splitting after the first and second dimension separation was utilized for volumetric flow reduction and for enabling a multi‐detector approach (with ultraviolet, fluorescence, charged aerosol, and MS detection), respectively. Derivatization with 6‐aminoquinolyl‐N‐hydroxysuccinimidyl carbamate provided a chromophore, a fluorophore, and an efficient mass tag for efficient ionization in positive electrospray ionization‐mass spectrometry. Chiral columns often have limitations in terms of their chemoselectivity, which may be a problem when complex sample mixtures with structurally related compounds need to be separated. It can be alleviated by a reversed‐phase×chiral two‐dimensional‐liquid chromatography setup, in which the first dimension provides the chemoselectivity and a chiral tandem column constituted of quinine‐carbamate derived weak anion‐exchanger and zwitterionic ion‐exchanger in the second dimension separation of D‐ and L‐amino acid enantiomers. The method was used to control the stereointegrity of the therapeutic peptide octreotide. After hydrolysis, all amino acid constituents were detected with the correct configuration and composition. Some options for flow splitting and integration of destructive detectors in the first dimension separation are outlined. [ABSTRACT FROM AUTHOR]

Time-of-flight mass spectrometry is a commonly mass spectrometry technique that is widely used in biomedicine, environmental science and food science. The multiple reflection time-of-flight (MR-TOF) mass analyzer is a new type of mass analyzer with ultra-high mass resolution and has been used at institutions, such as Helmholtz Centre for Heavy Ion Research (GSI), European Organization for Nuclear Research (CERN) and High Energy Accelerator Research Organization (KEK) to measure short-lived ion masses, separate isobar and store ions. As the demand for use increasing, it is becoming important to improve the resolving power of MR-TOF mass analyzers. However, the optimization of the voltage parameters of MR-TOF mass analyzers is a high-dimensional, highly refined and non-linear problem, which is difficult to solve optimally by analytical method. In this study, a particle swarm optimization (PSO) algorithm-based method for optimizing the voltage parameters of MR-TOF mass analyzers was proposed. The method used an improved particle swarm optimization (IPSO) approach with a inertia weight decay strategy. The optimization method was tested on the SIMION ion optics simulation platform. Considering 133Cs+ ion with E-1.5 keV, δE = 8.5 eV, δx = δy = 1 mm, δα = δβ 1.5 mrad, a mass resolving power over 8.1X105 was achieved when A=0 ns and a mass resolving power over 5.0X105 was achieved when Δt=20 ns. IPSO optimized the best results to achieve the 2nd order focus of time with respect to energy for the MR-TOF mass analyzer, and the deviation of the ion's half-turn time of flight was within 1. 3×10-6. In 20 times experiments. IPSO improved the maximum results by 33%, the average results by 35% and the standard deviation by 29% compared with PSO optimization, providing better solution quality and stability. IPSO's linear decay strategy effectively controlled the reduction of the voltage update step size and was able to meet the global search and refinement of the MR-TOF mass analyzer voltage parameter optimization problem. It had good convergence and convergence speed. This work provided a fast and effective method for optimizing the voltage parameters of the MR-TOF mass analyzer and helped to improve the performance of this analyzer. The results showed that the IPSO is able to obtain a limiting mass resolution of more than 810 000, which has better performance compared with the PSO. The method has the advantages of simple operation, fast optimization and better solution, which can provide a method reference for voltage optimization of MR-TOF mass analyzer and thus improve the development efficiency of MR-TOF mass analyzer. [ABSTRACT FROM AUTHOR]

Sterones are one of the active components of Achyranthes bidentata, and the difficulty in distinguishing sterone isomers poses a great challenge to the accurate identification of the chemical components of Achyranthes bidentata, while online energy-resolved mass spectrometry (Online ER-MS) has been proved to be an effective method for distinguishing the isomers due to its ability to provide rich MS/MS fragment information. In this study, mass spectra of sterones were collected by ultra-high performance liquid chromatography-quadrupole tandem time-of-flight mass spectrometry (UHPLC- Q-TOF-MS/MS), and then the structures of the compounds were matched with MS/MS fragment ions to initially identify the sterone compounds in Achyranthes bidentata. In order to further distinguish the sterones isomers, the fragment ions with higher abundance detected in UHPLC-Q-TOF-MS/MS were selected to construct pseudoion transitions (PITs), and the collision energy (CE) and relative ion intensity of PITs were collected by using the multi-reaction monitoring mode of ultra-high performance liquid chromatography tandem quadrupole linear ion trap mass/mass spectrometry (UHPLC-Q-trap-MS/MS). Further, the relative ion intensity of each PIT under different CE was recorded, and the dataset was imported into GraphPad Prism software to draw the fragmentation curve for each ion transition via Gaussian fitting. The vertex of the fragmentation curve was defined as the optimal collision energy (OCE), and the OCE of differention transitions of each compound was calculated respectively. At the same time. combined with quantum structural calculation, the thermal enthalpies of precursor ions and product ions in each candidate structure were calculated using Gaussian program based on density functional theory, and the bond energy required to break the corresponding chemical bond was calculated according to the difference between the precursor ion and the two product ions. The OCE and bond energies of each group of isomers were analyzed to establish the relationship between the chemical structure and OCE. The results showed that the energy required to break the same chemical bond was not the same due to the different substituent positions of isomers, which made the OCE of different ion transitions of isomers also differ. Finally, 12 sterones including three groups of the isomers were identified from Achyranthes bidentata, and the feasibility of the method was verified by comparing with the standards. Therefore, the combination of online energy-resolved mass spectrometry and quantum structural calculation can achieve efficient differentiation of isomers, providing a new solution for accurate identification of isomers in traditional Chinese medicines. [ABSTRACT FROM AUTHOR]

An efficient strategy for the identification of potential nephroprotective substances in Zhu‐Ling decoction has been established with the integration of absorbed components characterization, pharmacokinetics, and activity evaluation. A qualitative method was developed to characterize the chemical constituents absorbed components in vivo of Zhu‐Ling decoction by using ultra‐performance liquid chromatography‐quadrupole‐time‐of‐flight mass spectrometry. A quantitative method was established and validated for the simultaneous determination of eight compounds in rat plasma by using ultra‐performance liquid chromatography‐triple quadruple tandem mass spectrometry. Finally, the nephroprotective activities of absorbed components with high exposure were assessed by cell survival rate, superoxide dismutase, and malondialdehyde activities in hydrogen peroxide–induced Vero cells. As a result, 111 compounds in Zhu‐Ling decoction and 36 absorbed components were identified in rat plasma and urine, and poricoic acid A, poricoic acid B, alisol A, 16‐oxo‐alisol A, and dehydro‐tumulosic acid had high exposure levels in rat plasma. Finally, poricoic acid B, poricoic acid A, 16‐oxo‐alisol A, and dehydro‐tumulosic acid showed remarkable nephroprotective activity against Vero cells damage induced by hydrogen peroxide. Besides, superoxide dismutase and malondialdehyde activities were obviously regulated in hydrogen peroxide–induced Vero cells by treatment with the four compounds mentioned above. Therefore, these four compounds were considered to be effective substances of Zhu‐Ling decoction due to their relatively high exposure in vivo and biological activity. This study provided a chemical basis for the action mechanism of Zhu‐Ling decoction in the treatment of chronic kidney diseases. [ABSTRACT FROM AUTHOR]

Aconitum carmichaelii is widely used to treat chronic and intractable diseases due to its remarkable curative effect, but it is also a highly toxic herb with severe cardiac and neurotoxicity. It has been combined with honey for thousands of years to reduce toxicity and enhance efficacy, but there has been no study on the chemical constituent changes in the honey‐processing so far. In this study, the chemical constituents of A. carmichaelii before and after honey‐processing were characterized by ultra‐high‐performance liquid chromatography‐quadrupole time‐of‐flight tandem mass spectrometry. The results showed that a total of 118 compounds were identified, of which six compounds disappeared and five compounds were newly produced after honey‐processing, and the cleavage pathway of main components was elucidated. At the same time, 25 compounds were found to have significant effects on different products, among which four compounds with the biggest difference were selected for quantitative analysis by ultra‐high‐performance liquid chromatography‐tandem mass spectrometry. This study not only explained the chemical differences between the different products, but also helped to control the quality of the honey‐processed products more effectively, and laid a foundation for further elucidating the mechanism of chemical constituent change during the honey‐processing of A. carmichaelii. [ABSTRACT FROM AUTHOR]

Fuzhuan brick tea, a distinctive dark tea fermented by microorganisms, is a traditional beverage in China throughout history. Recently, it has attracted considerable attention owing to its unique quality characteristics and potential health benefits. The aim of this study was to establish a method for the quality control of Fuzhuan brick tea for stable production. Ultra‐high‐performance liquid chromatography coupled with quadrupole time‐of‐flight tandem mass spectrometry was used to identify Fuzhuan brick tea, and the major components were chosen for further quantitative analysis. Subsequently, a quantification method was developed using ultra‐high‐performance liquid chromatography coupled with triple‐quadrupole mass spectrometry, and its reliability was verified through methodological validation. Finally, a total of 30 compounds were identified, including catechins, flavonoids, alkaloids, and fatty acids. The established method was reliable for methodological validation and was applied to the quantitative analysis of Fuzhuan brick tea. This study provides a fundamental basis for the quality control and further studies on the component analysis of Fuzhuan brick tea. [ABSTRACT FROM AUTHOR]

The rhizome of Atractylodes lancea (Thunb.) DC. (AL), called Maocangzhu in Chinese, is a geoherbalism medical herb in Jiangsu Province that is often used in the prescription of traditional Chinese medicine (TCM), such as for the treatment of COVID-19. The landform and climatic environment of each province varies greatly from south to north, which has an important influence on the chemical constituents in AL. However, there is a lack of research on the significance of its geoherbalism, especially in water-soluble parts other than volatile oil. In this study, eight known compounds were isolated and obtained as reference substances from AL. In addition, liquid chromatography coupled with triple-quadrupole time-of-flight tandem mass spectrometry (LC-triple TOF-MS/MS) and gas chromatography–mass spectrometry (GC-MS) were used to analyze and characterize chemical constituents from different habitats. Moreover, orthogonal partial least-squares discriminant analysis (OPLS-DA) was applied to reveal the differential metabolomics in AL from different habitats based on the qualitative information of the chemical constituents. Results showed that a total of 33 constituents from GC-MS and 106 constituents from LC-triple TOF-MS/MS were identified or inferred, including terpenoids, polyacetylenes, and others; meanwhile, the fragmentation pathways of different types of compounds were preliminarily deduced from the fragmentation behavior of the major constituents. According to the variable importance in projection (VIP) and p-values, only one volatile differential metabolite was identified by GC-MS screening: β-eudesmol. Overall, five differential metabolites were identified by LC-triple TOF-MS/MS screening: sucrose, 4(15),11-eudesmadiene; atractylenolide I, 3,5,11-tridecatriene-7,9-diyne-1,2-diacetate, and (3Z,5E,11E)-tridecatriene-7,9-diynyl-1-O-(E)-ferulate. This study provides metabolomic information for the establishment of a comprehensive quality evaluation system for AL. [ABSTRACT FROM AUTHOR]

The vast pool of structurally and functionally distinct secondary metabolites (i.e., natural products (NPs)) is constantly being expanded, a process also driven by the rapid progress in the development of analytical techniques. Such NPs often show potent biological activities and are therefore prime candidates for drug development and medical applications. The ethyl acetate extract of the tuber of Citrullus naudinianus (C. naudinianus), an African melon with edible fruits and seeds, shows in vitro immunomodulatory activity presumably elicited by cucurbitacins that are known major constituents of this plant. Further potentially immunomodulatory cucurbitacins or cucurbitacin derivatives were assumed to be in the tuber. Given the typically high content of cucurbitacins with similar physicochemical features but often distinct bioactivities, an efficient and reliable separation process is a prerequisite for their detailed characterization and assessment in terms of bioactivity. We therefore developed a detection method to screen and differentiate cucurbitacins via high-performance liquid chromatography/quadrupole-time-of-flight tandem mass spectrometry (HPLC-QTOF-MS/MS). In order to confirm the identification, the fragmentation patterns of two cucurbitacins and one 23,24-dihydrocucurbitacin were also investigated. Six characteristic fragments were identified and three of them were employed for the identification of cucurbitacins and 23,24-dihydrocucurbitacins in the extract. As a result, in addition to eight previously reported cucurbitacins from this plant four distinct 23,24-dihydrocucurbitacins (B, D, E, and I) were putatively identified and newly found in the ethyl acetate extract of the tuber of C. naudinianus. The established methodology enables rapid and efficient LC-MS-based analysis and identification of cucurbitacins and 23,24-dihydrocucurbitacins in plant extracts. [ABSTRACT FROM AUTHOR]

Mammalian plasma kallikrein (PK) and coagulation factor XI (fXI) are serine proteases that play in the kinin–kallikrein cascade and in the blood clotting pathway. These proteases share sequence homology and have four apple domains (APDs) and a serine protease domain (SPD) from their N-terminus to C-terminus. No homologs of these proteases are believed to be present in fish species, except for lobe-finned fish. Fish, however, have a unique lectin, named kalliklectin (KL), which is composed of APDs only. In the present study, we found genomic sequences encoding a protein with both APDs and SPD in a few cartilaginous and bony fishes, including the channel catfish Ictalurus punctatus, using bioinformatic analysis. Furthermore, we purified two ~ 70 kDa proteins from the blood plasma of the catfish using mannose-affinity and gel filtration chromatography sequentially. Using de novo sequencing with quadrupole time-of-flight tandem mass spectrometry, several internal amino acid sequences in these proteins were mapped onto possible PK/fXI-like sequences that are thought to be splicing variants. Exploration of APD-containing proteins in the hagfish genome database and phylogenetic analysis suggested that the PK/fXI-like gene originated from hepatocyte growth factor, and that the gene was acquired in a common ancestor of jawed fish. Synteny analysis provided evidence for chromosomal translocation around the PK/fXI-like locus that occurred in the common ancestor of holosteans and teleosts after separation from the lobe-finned fish lineage, or gene duplication into two chromosomes, followed by independent gene losses. This is the first identification of PK/fXI-like proteins in teleosts. [ABSTRACT FROM AUTHOR]

Six sartan substances including telmisartan, losartan, valsartan, irbesartan, olmesartan, and candesartan were selected in this work. A simple and sensitive liquid chromatography–tandem mass spectrometry method was developed and validated to simutaniously detect six drugs. Linearity, LOD, and LOQ were satisfied for routine quantitative and qualitative detection. The linearity ranged from 2 to 1000 ng/mL with the determination coefficient more than 0.98. The intra-day and inter-day precisions were all below 27.5%. All the recoveries were above 80%, and matrix effects were between 25 and 120%. Profiling detection of six sartan substances in human urine was also developed after administration. Irbesartan urinary metabolic pathway was firstly investigated by liquid chromatography quadruple time-of-flight mass spectrometry using full scan and targeted tandem mass spectrometry techniques. Fifteen urinary metabolites of irbesartan were identified and characterized, and ten of them were firstly reported. [ABSTRACT FROM AUTHOR]

Cancer remains the second most common cause of death after cardiovascular diseases, accounting for nearly 10 million deaths in 2020. Although the incidence of cancer increases considerably with age, the cancer burden can also be reduced and have a high chance of cure through early detection, appropriate treatment, and care of patients. The development of high-throughput analytical approaches, like matrix-assisted laser desorption/ionization time-of-flight mass spectrometry (MALDI-TOF MS), contributes to identifying a pool of proteins/peptides as putative biomarkers for the early detection, diagnosis, and tumor progression. The purpose of the current review is to present an updated outline of recent proteome/peptidome research to establish putative cancer biomarkers using MALDI-TOF MS and highlight the applicability of statistical analysis in the oncology field. The pros and cons of MALDI-TOF MS application on cancer diagnostics and monitoring will be discussed, as well as compared with tandem mass spectrometry (MS/MS)-based proteomics (e.g., liquid chromatography–tandem mass spectrometry). In addition, pre-analytical (e.g., sample quality control) and analytical (e.g., sample pre-treatment, instrumental analytical conditions) properties that influence the robustness of MALDI-TOF MS data will be also discussed. [ABSTRACT FROM AUTHOR]

Legumes contain dietary fiber and resistant starch, which are beneficial to the intestinal environment. Here, we investigated the effects of yellow pea noodle consumption on the gut microbiota and fecal metabolome of healthy individuals. This single‐armed pre‐post comparative pilot study evaluated eight healthy female participants who consumed yellow pea noodles for 4 weeks. The gut microbiota composition and fecal metabolomic profile of each participant were evaluated before (2 weeks), during (4 weeks), and after (4 weeks) daily yellow pea noodle consumption. 16S rRNA gene sequencing was performed on stool samples, followed by clustering of operational taxonomic units using the Cluster Database at High Identity with Tolerance and integrated QIIME pipeline to elucidate the gut microbiota composition. The fecal metabolites were analyzed using capillary electrophoresis time‐of‐flight mass spectrometry and liquid chromatography time‐of‐flight mass spectrometry. Compared to day 0, the relative abundances of five bacterial genera (Bacteroides, Bilophila, Hungatella, Parabacteroides, and Streptococcus) in the intestinal microbiota significantly decreased, wherein those of Bifidobacterium longum and Ruminococcus bromii were increased on day 29 and decreased to the basal level (day 0) on day 57. Fecal metabolomic analysis identified 11 compounds showing significant fluctuations in participants on day 29 compared to day 0. Although the average levels of short‐chain fatty acids in participants did not differ significantly on day 29 compared to those on day 0, the levels tended to increase in individual participants with >8% relative abundance of R. bromii in their gut microbiota. In conclusion, incorporating yellow peas as a daily staple may confer human health benefits by favorably altering the intestinal environment. [ABSTRACT FROM AUTHOR]

Flavonoids have been attracting increasing research interest because of their multiple health promoting effects. However, many flavonoids with similar structures are present in foods, often at low concentrations, which increases the difficulty of their separation and identification. Liquid chromatography-quadrupole time-of-flight tandem mass spectrometry (LC-Q-TOF-MS/MS) has become one of the most widely used techniques for flavonoid detection. LC-Q-TOF-MS/MS can achieve highly efficient separation by LC; it also provides structural information regarding flavonoids by Q-TOF-MS/MS. This review presents a comprehensive summary of the scientific principles and detailed methodologies (e.g., qualitative determination, quantitative determination, and data processing) of LC-Q-TOF-MS/MS specifically for food flavonoids. it also discusses the recent applications of LC-Q-TOF-MS/MS in determination of flavonoid types and contents in agricultural products, changes in their structures and contents during food processing, and metabolism in vivo after consumption. Moreover, it proposes necessary technological improvements and potential applications. This review would facilitate the scientific understanding of theory and technique of LC-Q-TOF-MS/MS for flavonoid detection, and promote its applications in food and health industry. [ABSTRACT FROM AUTHOR]

Rationale: Gas chromatography–mass spectrometry (GC–MS) is the most frequently applied technique for analyzing Amaryllidaceae alkaloids in plant extracts. Having these compounds, known for their potent bioactivities, is a distinctive chemotaxonomic feature of the Amaryllidoideae subfamily (Amaryllidaceae). The Amaryllidaceae alkaloids of homolycorine type with a C3–C4 double bond generally show molecular and diagnostic ions at the high‐mass region with low intensity in the EIMS mode, leading to problematic identification in complex plant extracts. Methods: Eleven standard homolycorine‐type alkaloids (isolated and identified by 1D and 2D nuclear magnetic resonance) were subjected to separation with GC and studied with electron impact mass spectrometry (EIMS) including single quadrupole (GC–EIMS), tandem (GC–EIMS/MS), and high‐resolution (GC–HR‐EIMS) detectors, as well as with chemical ionization mass spectrometry (GC–CIMS). Alkaloid fractions from two Hippeastrum species and Clivia miniata were subjected to GC–EIMS and GC–CIMS for alkaloid identification. Results: GC–EIMS in combination with GC–CIMS provided significant structural information of homolycorine‐type alkaloids with C3–C4 double bond, facilitating their unambiguous identification. Based on the obtained typical fragmentation, other 11 homolycorine‐type compounds were identified in extracts from two Hippeastrum species by parallel GC–EIMS, GC–CIMS, and liquid chromatography–electrospray ionization time‐of‐flight mass spectrometry and in extracts from C. miniata by GC–EIMS. Conclusions: GC–MS can be successfully applied for the identification of new and known homolycorine‐type alkaloids, among others within the Amaryllidoideae subfamily, as well as for chemotaxonomical and chemoecological studies. [ABSTRACT FROM AUTHOR]

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Dioscorea opposita Thunb., a traditional medicinal and food homologous plant, has been used for thousands of years in folk medicine and nutritious food, partially due to the metabolites. However, detailed information on the metabolites in Dioscorea opposita Thunb. peel is still scarce. Herein, an ultra‐high‐performance liquid chromatography‐quadrupole/orbitrap high‐resolution mass spectrometry‐based metabolomics approach was used to reveal the comprehensive metabolites in Dioscorea opposita Thunb. peel. The proposed method provided tentative identification of 307 metabolites. Among them, 286 metabolites are reported herein in Dioscorea opposita Thunb. peel for the first time, namely: 87 lipids, 49 phenolic acids, 34 flavonoids, 29 amino acids and derivatives, 28 organic acids, 14 alkaloids, 10 lignans, and coumarins, eight saccharides and vitamins, six nucleotides and derivatives, two quinones, and 19 others. The obtained results highlight the importance of Dioscorea opposita Thunb. peel as a promising source of bioactive ingredients, and form a basis for future quantitative and bioavailability studies. [ABSTRACT FROM AUTHOR]

Trachyspermum ammi (L.) Sprague (Apiaceae), commonly known as "Ajwain" is distributed throughout India. Ajwain fruits contain fiber, carbohydrates, phenolic acids, flavonoids, and tannins. The fruits also yield a small amount of essential oil, with Thymol as the principal constituent. Ajwain has various pharmacological activities like anti‐leishmanial, antimicrobial, cytotoxic, antispasmodic, nematocidal, and anthelmintic. The fruits are of high therapeutic value; thus, it becomes quite essential to evaluate the quality of Trachyspermum ammi (L.) Sprague to authenticate and ensure its therapeutic and nutritional properties. The ethyl acetate fraction of Trachyspermum ammi (L.) Sprague fruits exhibited the highest total phenolic and flavonoid content values of 149.55 ± 1.19 mg rutin equivalent and 682.85 ± 3.68 mg gallic acid equivalent, respectively. Metabolite profiling of the ethyl acetate fraction using ultra‐performance liquid chromatography‐quadrupole time‐of‐flight tandem mass spectrometry analysis resulted in identifying 19 phytomolecules. A validated high‐performance thin‐layer chromatography method was developed to quantify standard phytomolecules in the ethyl acetate fraction. The highest and lowest percentages of phytomarker were found to be caffeic acid (5.51% ± 0.16% w/w) and gallic acid (1.29% ± 0.09% w/w), respectively. This validated rapid, accurate, and precise method for standardization of Trachyspermum ammi (L.) Sprague will be beneficial for its quality evaluation as well as the derived products. [ABSTRACT FROM AUTHOR]