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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 (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 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]

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 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]

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]

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]

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]