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The constituents and antioxidant activities of Cyperus exaltatus var. iwasakii (CE) have not been studied to date. In this study, the 2,2-diphenyl-1-picrylhydrazyl (DPPH) and 2,2′-azino-bis(3-ethylbenzothiazoline-6 sulfonic acid) (ABTS) assays were used to evaluate the radical-scavenging activities of the ethanol extract, four fractions, and isolated compounds of CE. In addition, phenolic acids and flavonoids were isolated from the ethanol extract of CE using column chromatography. The compounds identified by spectroscopy were gallic acid, protocatechuic acid, vanillic acid, p-coumaric acid, rutin, ferulic acid, isoquercitrin, astragalin, quercetin, luteolin, apigenin, tricin, and kaempferol. Quantitative analysis using high-performance liquid chromatography (HPLC) revealed that the major flavonoids of CE were astragalin and tricin and that the major phenolic acid was p-coumaric acid. In addition, comparative analysis of CE from Ganghwa and Hampyeong habitats using HPLC showed that the Hampyeong CE had a higher phytochemical content. Comparative analyses of the isolated compounds were also conducted among five Cyperus species. The highest antioxidant activities were found in the ethyl acetate (EtOAc) fraction, and among the compounds isolated from CE, vanillic acid and quercetin showed remarkable antioxidant activity even when compared with ascorbic acid. The results demonstrate the usefulness of CE, which has not been sufficiently studied previously, and will facilitate the evaluation of its potential effectiveness as antioxidant functional plant material. [ABSTRACT FROM AUTHOR]

Bee pollen, known as a 'life-giving dust', is a product of honeybees using flower pollen grains and combining them with their saliva secretions. Thus, flower pollen could be an indicator of the bee pollen botanical source. Identification of bee pollen sources is a highly crucial process for the evaluation of its health benefits, as chemical composition is directly related to its pharmacological activity. In this study, the chemical profiles, contents of phenolic marker compounds and pharmacological activities of Hedera helix L. (ivy) bee pollen samples from Türkiye and Slovenia, as well as ivy flower pollen grains, were compared. High-performance thin-layer chromatography (HPTLC) analyses revealed that pollen samples, regardless of where they were collected, have similar chemical profiles due to the fact that they have the same botanical origins. Marker compounds afzelin, platanoside and quercetin-3-O-β-glucopyranosyl-(1→2)-β-galactopyranoside, common to both bee pollen and flower pollen, were isolated from bee pollen, and their structures were elucidated by nuclear magnetic resonance (NMR) and mass spectrometry (MS). These three compounds, as well as chlorogenic acid and 3,5-dicaffeoylquinic acid (found in flower pollen), were quantified using high-performance liquid chromatography (HPLC) analyses. In vitro tests and effect-directed analyses were used to evaluate the xanthine oxidase inhibition and antioxidant activity of the marker compounds and extracts from flower pollen and bee pollen. This is the first report comparing chemical profiles and related bioactivities of the flower pollen and bee pollen of the same botanical origin, as well as the first report of the chemical profile and related bioactivities of ivy flower pollen. [ABSTRACT FROM AUTHOR]

Zanthoxylum nitidum (Roxb.) DC. (ZN), with strong effects of anti-inflammation and antioxidant activities is treated as a core herb in traditional Chinese medicine (TCM) preparation for treating stomachache, toothache, and rheumatoid arthritis. However, the active ingredients of ZN are not fully clarified due to its chemical complexity. In the present study, a double spectrum–effect analysis strategy was developed and applied to explore the bioactive components in herbs, and ZN was used as an example. Here, the chemical components in ZN were rapidly and comprehensively profiled based on the mass defect filtering-based structure classification (MDFSC) and diagnostic fragment-ion-based extension approaches. Furthermore, the fingerprints of 20 batches of ZN samples were analyzed by high-performance liquid chromatography, and the anti-inflammatory and antioxidant activities of the 20 batches of ZN samples were studied. Finally, the partial least squares regression (PLSR), gray relational analysis models, and Spearman's rank correlation coefficient (SRCC) were applied to discover the bioactive compounds in ZN. As a result, a total of 48 compounds were identified or tentatively characterized in ZN, including 35 alkaloids, seven coumarins, three phenolic acids, two flavonoids, and one lignan. The results achieved by three prediction models indicated that peaks 4 , 12 , and 17 were the potential anti-inflammatory compounds in ZN, whereas peaks 3 , 5 , 7 , 12 , and 13 were involved in the antioxidant activity. Among them, peaks 4 , 5 , 7 , and 12 were identified as nitidine, chelerythrine, hesperidin, and oxynitidine by comparison with the standards and other references. The data in the current study achieved by double spectrum–effect analysis strategy had great importance to improve the quality standardization of ZN, and the method might be an efficiency tool for the discovery of active components in a complex system, such as TCMs. [ABSTRACT FROM AUTHOR]

Forsythia suspensa (Thunb.) Vahl (F. suspensa) is a traditional Chinese medical herb and only its fruit is currently used in clinical therapies. However, the discarded parts like leaves also contain a large number of active components. In this study, we used macroporous adsorption resin to enrich the effective components from F. suspensa leaves. The separated active compounds were then identified and quantified by ultra-performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (UPLC/Q-TOF MS) and high-performance liquid chromatography Active components with antibacterial properties extracted from F. suspensa leaves were confirmed in vitro and the corresponding mechanisms were explored. In sum, a stable and effective method for extracting antibacterial active components from F. suspensa leaves was established in this study, which proved the practicability of F. suspensa leaves as traditional Chinese medicine and is conducive to the more comprehensive utilization of the plant. [ABSTRACT FROM AUTHOR]

Zilongjin tablets as a traditional Chinese medicine are widely used for primary lung cancer patients with deficiency of "qi " and "blood " syndrome undergoing chemotherapy. It is a compound preparation that consists of eight herbs. To clarify the chemical profiling of Zilong Jin tablets rapidly, a feasible and accurate strategy was developed by the ultra high performance liquid chromatography‐quadrupole/orbitrap high resolution mass spectrometry. According to the accurate mass and fragment ion information provided by high resolution mass spectrometry, the compounds were reasonably identified. In total, 74 compounds were characterized, including 20 flavonoids, 14 quinones, 15 organic acids, 6 phthalide compounds, and 19 other compounds. Among them, 34 major compounds were unambiguously confirmed by comparing with reference standards. This study could provide an important scientific basis for further research on quality control, pharmacokinetics and pharmacodynamics, and clinical application of Zilong Jin tablets. [ABSTRACT FROM AUTHOR]

Artemisia gmelinii Web. ex Stechm. (AG), a popular medicinal herb in Asia, has been used as a common food ingredient in Korea and is traditionally known for its anti-inflammatory properties. Therefore, in this study, we aimed to investigate whether AG relieves IBD, a classic chronic inflammatory disease of the gastrointestinal tract. We identified 35 chemical compounds in AG ethanol extract using ultra-high-performance liquid chromatography-quadrupole time-of-flight tandem mass spectrometry. In mice with DSS-induced IBD, AG administration attenuated the disease activity index and the serum and colonic levels of inflammatory cytokines and chemokines. AG treatment decreased nuclear factor- κ B (NF- κ B) signaling, a key mediator of inflammation, in the mouse colons. Additionally, AG extract enhanced immune responses in lymphoid tissues such as spleen and Peyer's patches. Thus, AG consumption potently ameliorated IBD symptoms and improved immune signaling in lymphoid tissues. [ABSTRACT FROM AUTHOR]

Clarification of the quality and biological effect equivalence of traditional Chinese medicines containing multi‐origin species is essential to improve their current quality standards, and also is the core problem to clarify the origins of single herbs with multi‐species in Chinese formulas that will guarantee their clinical application. Huangqin decoction is the typical one of multi‐origin formulas frequently used in traditional Chinese medicine and Kampo medicine. An ultra high performance liquid chromatography with electrospray ionization–tandem mass spectrometry was developed for chemical profiling and marker quantification of Huangqin decoction prepared with two different original types of peony root, white and red peony root. Forty‐seven main peaks in chemical profiling of Huangqin decoction prepared with white and red peony root were identified: nine were from peony root, 20 from baical skullcap root, 17 from licorice root, and one from jujubae fruit. The markers characteristics of the respective types of peony root in Huangqin decoction differ from that in single herbs, especially in terms of monoterpenoids and hydrolysable tannins. Subsequently, 17 representative markers in Huangqin decoction prepared with three types of peony root and their chemical characteristics and content distribution were carried out. [ABSTRACT FROM AUTHOR]

This is the first report on identification of all B-type proanthocyanidins from monomers to decamers (monomers—flavan-3-ols, dimers, trimers, tetramers, pentamers, hexamers, heptamers, octamers, nonamers, and decamers) and some of their gallates in leaves of Japanese knotweed (Fallopia japonica Houtt.), giant knotweed (Fallopia sachalinensis F. Schmidt) and Bohemian knotweed (Fallopia × bohemica (Chrtek & Chrtkova) J.P. Bailey). Flavan-3-ols and proanthocyanidins were investigated using high performance thin-layer chromatography (HPTLC) coupled to densitometry, image analysis, and mass spectrometry (HPTLC–MS/MS). All species contained (−)-epicatechin and procyanidin B2, while (+)-catechin was only detected in Bohemian and giant knotweed. (−)-Epicatechin gallate, procyanidin B1 and procyanidin C1 was only confirmed in giant knotweed. Leaves of all three knotweeds have the same chemical profiles of proanthocyanidins with respect to the degree of polymerization but differ with respect to gallates. Therefore, chromatographic fingerprint profiles of proanthocyanidins enabled differentiation among leaves of studied knotweeds, and between Japanese knotweed leaves and rhizomes. Leaves of all three species proved to be a rich source of proanthocyanidins (based on the total peak areas), with the highest content in giant and the lowest in Japanese knotweed. The contents of monomers in Japanese, Bohemian and giant knotweed were 0.84 kg/t of dry weight (DW), 1.39 kg/t DW, 2.36 kg/t, respectively, while the contents of dimers were 0.99 kg/t DW, 1.40 kg/t, 2.06 kg/t, respectively. Giant knotweed leaves showed the highest variety of gallates (dimer gallates, dimer digallates, trimer gallates, tetramer gallates, pentamer gallates, and hexamer gallates), while only monomer gallates and dimer gallates were confirmed in Japanese knotweed and monomer gallates, dimer gallates, and dimer digallates were detected in leaves of Bohemian knotweed. The profile of the Bohemian knotweed clearly showed the traits inherited from Japanese and giant knotweed from which it originated. [ABSTRACT FROM AUTHOR]

Glechomae Herba is a traditional Chinese medicine used for the treatment of urolithiasis, cholelithiasis, and urinary tract infections in China. Identification of chemical constituents is helpful to discover the potential active ingredients. However, this significant work is stymied by complex chemical constituents. Therefore, an ultra high performance liquid chromatography coupled to quadrupole‐time‐of‐flight tandem mass spectrometry analysis with diagnostic product ions and neutral loss filtering strategy was established for chemical profiling of Glechomae Herba. The diagnostic product ions and neutral loss filtering strategy simplified spectral elucidation. A total of 120 compounds, including 10 chlorogenic acids, 10 gallic acids, 21 phenylpropionic acids, and 77 flavonoids, were reasonably identified in Glechomae Herba. Sixty‐five constituents were first discovered in Glechomae Herba. Four types of chlorogenic acids (caffeoylquinic acid, feruloylquinic acid, p‐coumaroylquinic acid, and di‐caffeoylquinic acid), three types of galloylglucoses (di‐O‐galloyl‐glucose, tri‐O‐galloyl‐glucose, and tetra‐O‐galloyl‐glucose), three types of phenylpropionic acid skeletons (p‐coumaric acid, caffeic acid, and rosmarinic acid) and five types of flavonoid aglycone skeletons (apigenin, kaempferol, luteolin, quercetin, and chrysin) were identified in Glechomae Herba. The results indicated that the developed strategy was feasible and rational technique for identifying the complex chemical constituents in Glechomae Herba. [ABSTRACT FROM AUTHOR]

Tan Re Qing (TRQ), a traditional Chinese medicine formula, is composed of Scutellariae Radix and other four herbs (bear bile powder, Caprae Hircus Cornu, Lonicerae japonicae Flos and Forsythiae Fructus) used for the treatment of bronchitis and upper respiratory infection. Chemical constituents in the herb always changed in content during processing. So, in this study, the ingredient change was monitored from three froms of Scutellariae Radix, including original herb, intermediate and product (TRQ capsules) with the same batch by HPLC MS/MS. A total of 98 compounds, including 69 flavonoids, 5 phenylethanoid glucosides, 6 other compounds and 18 unknown components, were tentatively identified in Scutellariae Radix. Most minor components in Scutellariae Radix were disappeared during preparation process, and only 17 of these compounds were detected in TRQ capsules. 5,2'-Dihydroxy-7,8-dimethoxyflavone and one unknown compound were detected in the original herb and intermediate, but disappeared in the TRQ capsules. These findings indicated the productive process control is vital for risk assessment and chemical material basis, as well as the basis for quality control of TRQ capsules. [ABSTRACT FROM AUTHOR]

Platycladi Cacumen (PC) is a traditional Chinese medicine used for the treatment of hemorrhages, cough, asthma and hair loss. To get a better understanding of the chemical constituents in PC, ultra-high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UPLC-Q-TOF-MS/MS) and diagnostic ion filtering strategy were firstly employed for chemical profiling of PC. A total of 43 compounds including organic acids and derivatives, flavonoids as well as phenylpropanolds were unambiguously or reasonably identified. Coumarin and lignan were reported for the first time in PC. Chemical variation of 39 batches of PC from different geographical origins and 10 batches of processed product of PC was subsequently investigated by quantitation of nine major flavonoids. The results determined by UPLC coupled with diode array detection (UPLC-DAD) and hierarchical cluster analysis (HCA) indicated that the contents of flavonoids in PC samples differ greatly. This work provides an efficient approach to comprehensively evaluate the quality of PC. [ABSTRACT FROM AUTHOR]

In this study, a systematic data acquisition and mining strategy aimed at the traditional Chinese medicine (TCM) complex system based on ultra high-performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (UHPLC-Q-TOF-MS) was reported. The workflow of this strategy is as follows: First, the high resolution mass data are acquired by both data-dependent acquisition mode (DDA) and data-independent acquisition mode (DIA). Then a global data mining that combined targeted and non-targeted compound finding is applied to analyze mass spectral data. Furthermore, some assistant tools, such as key product ions (KPIs), are employed for compound hunting and identification. The TCM Ziwan (ZW, Aster tataricus rhizoma) was used to illustrate this strategy for the first time. In this research, total 131 compounds including organic acids, peptides, terpenes, steroids, flavonoids, coumarins, anthraquinones and aldehydes were identified or tentatively characterized in ZW based on accurate mass measurements within ±5 ppm error, and 50 of them were unambiguously confirmed by comparing standard compounds. Afterwards, based on the traditional Chinese medical theory and the key determinants of firing patterns of ventral tegmental area (VTA) dopamine (DA) neurons in the development of depression, the confirmed compounds were subsequently evaluated the pharmacological effect of activity of VTA DA neurons and anti-depressive efficacy. This research provided not only a chemical profiling for further in vivo study of ZW, but also an efficient data acquisition and mining strategy to profile the chemical constituents and find new bioactive substances for other TCM complex system. [ABSTRACT FROM AUTHOR]

Ultra-high-performance liquid chromatography coupled with quadrupole/time-of-flight mass spectrometry (UHPLC-Q/TOF-MS) in positive ion mode was used to profile and identify the major constituents in Euphorbia fischeriana Steud. ( E . fischeriana ). An Agilent ZORBAX SB-C 18 column was used to separate the crude extract of E . fischeriana , and the mobile phases were acetonitrile and 0.1% aqueous formic acid (v/v). A total of 40 peaks were detected, and 37 components, including phloroglucinol derivatives, diterpenoids and nitrogenous compounds, were identified based on their accurate masses and fragmentation characteristics. The chemical structures of 7 of the detected compounds were determined by comparing standard compounds to the compounds that were isolated from E . fischeriana . Reasonable fragmentation mechanisms and key fragment ions of the four jolkinolide components were determined to aid in the identification of the other diterpenoids in E. fischeriana . In addition, the compound corresponding to peak 18, namely, jolkinomethylide, was determined to be new, and its chemical structure was determined and elucidated based on MS and NMR spectroscopic data. The present study provided valuable information on the new components in E. fischeriana and established a practical method for evaluating the quality of E. fischeriana . [ABSTRACT FROM AUTHOR]

ShenKang injection is traditional Chinese medicine used to treat chronic renal failure in China. It is a compound preparation that consists of four herbs: Rhubarb, Salvia miltiorrhiza, Safflower and Radix Astragali. We developed an ultra high pressure liquid chromatography coupled with Q Exactive hybrid quadrupole-orbitrap high resolution accurate mass spectrometry tandem mass spectrometry method to analyze its chemical compositions, and a total of 90 compounds were identified from ShenKang injection. Among them, 19 major compounds were unambiguously detected by comparing with reference standards. Meanwhile, 13 representative compounds selected as quality control markers were simultaneously quantified in ShenKang injection samples. Chromatographic separation was accomplished on a Waters ACQUITY HPLC® HSS C18 column using gradient elution. The method was validated with respect to linearity, sensitivity, accuracy and precision, reproducibility and stability. And the validated method was successfully applied for simultaneous determination of 13 bioactive compounds in ShenKang injection from ten batches of samples by liquid chromatography with mass spectrometry. The results were analyzed by principal components analysis method, and three compounds had a significant relationship with the quality control of ShenKang injection. This research established a rapid and reliable method for the integrating quality control, including qualitation and quantification of ShenKang injection. [ABSTRACT FROM AUTHOR]

An ultra high performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight mass spectrometry method in both positive and negative ion modes was established in order to comprehensively investigate the major constituents in Wu Ji Bai Feng Pill. Briefly, a Waters ACQUITY UPLC HSS C18 column was used to separate the aqueous extract of Wu Ji Bai Feng Pill. A total of 0.1% formic acid in acetonitrile and 0.1% aqueous formic acid v/v were used as the mobile phase. All analytes were determined using quadrupole time-of-flight mass spectrometry with electrospray ionization source in positive and negative ion modes. At length, a total of 173 components including flavones and their glycosides, monoterpene glycosides, triterpene saponins, phenethylalchohol glycosides, iridoid glycosides, phthalides, tanshinones, phenolic acids, sesquiterpenoids and cyclopeptides were identified or tentatively characterized in Wu Ji Bai Feng Pill in an analysis of 16.0 min based on the accurate mass and tandem mass spectrometry behaviors. The developed method is rapid and highly sensitive to characterize the chemical constituents of Wu Ji Bai Feng Pill, which could not only be used for chemical standardization and quality control of Wu Ji Bai Feng Pill, but also be helpful for further study in vivo metabolism of Wu Ji Bai Feng Pill. [ABSTRACT FROM AUTHOR]

Cimicifugae Rhizoma (Sheng ma) is a Ranunculaceae herb belonging to a composite family and well known in China. has been widely used in traditional Chinese medicine. The Pharmacopoeia of the People׳s Republic of China contains three varieties ( Cimicifuga dahurica (Turcz.), Cimicifuga foetida L. and Cimicifuga heracleifolia Kom.) which have been used clinically as “Sheng-ma”. However, the chemical constituents of three components of “Sheng-ma” have never been documented. In this study, a rapid method for the analysis of the main components of “Sheng-ma” was developed using ultra-high performance liquid chromatography with quadrupole-time-of-flight mass spectrometry (UPLC/Q-TOF-MS). The present study reveals the major common and distinct chemical constituents of C. dahurica , C. foetida and C. heracleifolia and also reports principal component and statistical analyses of these results. The components were identified by comparing the retention time, accurate mass, mass spectrometric fragmentation characteristic ions and matching empirical molecular formula with that of the published compounds. A total of 32 common components and 8 markers for different “Sheng-ma” components were identified. These findings provide an important basis for the further study and clinical utilities of the three “Sheng-ma” varieties. [ABSTRACT FROM AUTHOR]

Ethnopharmacological relevance Toad venom and toad skin have been widely used for treating various cancers in China. Bufadienolides are regarded as the main anticancer components of toad venom, but the difference on composition and anticancer activities of bufadienolides between toad venom and toad skin remains unclear. Methods Fractions enriched with free and conjugated bufadienolides were prepared from toad venom and toad skin. Bufadienolides in each fraction were comprehensively profiled by using a versatile UHPLC-TOF-MS method. Relative contents of major bufadienolides were determined by using three bufogenins and one bufotoxin as marker compounds with validated UHPLC-TOF-MS method. Furthermore, cytotoxicity of the fractions was examined by MTT assay. Results Two fractions, i.e. , bufogenin and bufotoxin fractions (TV-F and TV-C) were isolated from toad venom, and one bufotoxin fraction (TS-C) was isolated from toad skin. Totally 56 bufadienolides in these three fractions were identified, and 29 were quantified or semi-quantified. Bufotoxins were identified in both toad venom and toad skin, whereas bufogenins exist only in toad venom. Bufalin-3-conjugated bufotoxins are major components in toad venom, whereas cinobufotalin and cinobufagin-3-conjugated bufotoxins are main bufotoxins in toad skin. MTT assay revealed potent cytotoxicity of all the fractions in an order of TV-F>TV-C>TS-C. Conclusions Our study represents the most comprehensive investigation on the chemical profiles of toad venom and toad skin from both qualitative and quantitative aspects. Eight bufotoxins were identified in toad skin responsible for the cytotoxicity for the first time. Our research provides valuable chemical evidence for the appropriate processing method, quality control and rational exploration of toad skin and toad venom for the development of anticancer medicines. [ABSTRACT FROM AUTHOR]

The Kang-Jing (KJ) formula is a compound preparation made from 12 kinds of herbs. So far, four different methods (M1-M4) have been documented for KJ preparation, but the influence of preparation methods on the holistic quality of KJ have remained unknown. In this study, a strategy was proposed to investigate the influence of different preparation methods on the holistic quality of KJ using ultra-high performance liquid chromatography coupled with quadrupole/time of flight mass spectrometry (UHPLC-QTOF-MS/MS) based chemical profiling. A total of 101 compounds mainly belonging to flavonoids, tanshinones, monoterpene glycosides, triterpenoid saponins, alkaloids, phenolic acids and volatile oils, were identified. Among these compounds, glaucine was detected only in M3/M4 samples, while two dehydrocorydaline isomers merely detected in M2/M3/M4 samples. Tetrahydrocolumbamine, ethylic lithospermic acid, salvianolic acid E and rosmarimic acid were only detected in M1/M3/M4 samples. In the subsequent quantitative analysis, 12 major compounds were determined by UHPLC-MS/MS. The proposed method was validated with respect to linearity, accuracy, precision and recovery. It was found that the contents of marker compounds varied significantly in samples prepared by different methods. These results demonstrated that preparation method does significantly affect the holistic quality of KJ. UHPLC-QTOF-MS/MS based chemical profiling approach is efficient and reliable for comprehensive quality evaluation of KJ. Collectively, this study provide the chemical evidence for revealing the material basis of KJ, and establish a simple and accurate chemical profiling method for its quality control. [ABSTRACT FROM AUTHOR]

An ultra-high-performance liquid chromatography coupled with quadrupole-time-of-flight mass spectrometry (UHPLC–Q-TOF-MS) method was developed for the detection and structural analysis of ginsenosides in white ginseng and related processed products (red ginseng). Original neutral, malonyl, and chemically transformed ginsenosides were identified in white and red ginseng samples. The aglycone types of ginsenosides were determined by MS/MS as PPD ( m / z 459), PPT ( m / z 475), C-24, -25 hydrated-PPD or PPT ( m / z 477 or m / z 493), and Δ20(21)-or Δ20(22)-dehydrated-PPD or PPT ( m / z 441 or m / z 457). Following the structural determination, the UHPLC–Q-TOF-MS-based chemical profiling coupled with multivariate statistical analysis method was applied for global analysis of white and processed ginseng samples. The chemical markers present between the processed products red ginseng and white ginseng could be assigned. Process-mediated chemical changes were recognized as the hydrolysis of ginsenosides with large molecular weight, chemical transformations of ginsenosides, changes in malonyl-ginsenosides, and generation of 20-( R )-ginsenoside enantiomers. The relative contents of compounds classified as PPD, PPT, malonyl, and transformed ginsenosides were calculated based on peak areas in ginseng before and after processing. This study provides possibility to monitor multiple components for the quality control and global evaluation of ginseng products during processing. [ABSTRACT FROM AUTHOR]

Highlights: [•] Rapid and simultaneous quantification of lignans and amides is achieved by UPLC-DAD. [•] Different plant parts (leaves, bark, seeds) showed significant variation. [•] Tandem UPLC-DAD-ESI–MS/MS led to characterization of sixteen compounds. [•] Structural analysis by MS/MS and UV spectra is also discussed. [Copyright &y& Elsevier]

Abstract: Wu-tou decoction (WTD), a traditional Chinese medicine (TCM) formula, is composed of Aconiti Radix Cocta, Ephedrae Herba, Paeoniae Radix Alba, Astragali Radix and Glycyrrhiza Radix Preparata, and it has been used for more than a thousand years to treat rheumatic arthritis, rheumatoid arthritis and pain of joints, while the active constitutions of WTD are unclear. In this research, an ultra performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (UPLC–Q-TOF-MS) method in both positive and negative ion mode was established to investigate the major constitutions in WTD. A Waters ACQUITY UPLC BEH C18 column was used to separate the aqueous extract of WTD. Acetonitrile and 0.1% aqueous formic acid (v/v) were used as the mobile phase. 74 components including alkaloids, monoterpene glycosides, triterpene saponins, flavones and flavone glycosides were identified or tentatively characterized in WTD based on the accurate mass within 15ppm error and tandem MS behavior. All the constitutions were also detected in the corresponding individual herbs. These results will provide a basis for further study in vivo of WTD and the information of potential new drug structure for treating rheumatic arthritis and rheumatoid arthritis. [Copyright &y& Elsevier]

Highlights: [•] UPLC-PDA-Q/TOF–MS/MS approach for holistic quality evaluation of QYG. [•] 103 compounds were identified, of which 5 were generated during preparation of QYG. [•] Characteristic components were revealed for QYG samples prepared by three methods. [•] Preparation methods could significantly alter the holistic quality of QYG. [ABSTRACT FROM AUTHOR]

Abstract: A rapid, sensitive, and accurate HPLC-DAD method was developed and validated for simultaneous determination of one phenolic glycoside and seven monoterpene glycosides, including 1-O-β-d-(4-hydroxybenzoyl)glucose (1), pyridylpaeoniflorin (2), (8R)-piperitone-4-en-9-O-β-d-glucopyranoside (3), oxypaeoniflorin (4), 6′-O-β-glucopyranosylalbiflorin (5), albiflorin (6), β-gentiobiosylpaeoniflorin (7), and paeoniflorin (8), in 44 batches of peony seeds from nine Paeonia species collected from different areas. Using the optimised method, separations were conducted with a YMC-pack ODS-A column with water/formic acid and methanol as the mobile phase. All eight analytes demonstrated good linearity (r 2 >0.9993). The recoveries, measured at three concentration levels, varied from 98.20% to 103.81%. Six compounds including 1 and 4–8 occur ubiquitously in all the seeds of nine Paeonia species, and compounds 2 and 3 showed undetectable levels or very low content in several samples. The seed samples were classified into several groups, which coincide with the taxonomy of Paeonia at the section level. Peony seed might be a useful resource in developing new herbal or food products. [Copyright &y& Elsevier]

A rapid, sensitive, and accurate HPLC-DAD method was developed and validated for simultaneous determination of 10 stilbenes, which include suffruticosol A, suffruticosol B, suffruticosol C, resveratrol (E)-form,cis-ϵ-viniferin,trans-ϵ-viniferin,cis-suffruticosol D,cis-gnetin H,trans-suffruticosol D and gnetin H, in 44 plant samples from 9 differentPaeoniaspecies. In this optimized method, separations were carried out on an YMC-pack ODS-A column with water and methanol as mobile phase. The flow rate was set at 1.0 mL/min and the detector wavelength was set at 230 nm. The results showed that all the 10 analytes showed good linearity (r2 > 0.9994). The recoveries, measured at three concentration levels, varied from 97.19% to 102.89%. This method was also validated with respect to precision, repeatability, stability, and successfully applied to simultaneous determination of 10 stilbenes in 44 batches of peony seeds from 9Paeoniaspecies collected from different areas. [ABSTRACT FROM AUTHOR]

Abstract: Ethnopharmacological relevance: T. diversifolia (Hemsl.) A. Gray (Asteraceae) has been used in the traditional medicine in several countries as anti-inflammatory and against other illnesses. It is important to evaluate the anti-inflammatory activity of extracts from the leaves of this species, including an infusion, to identify the main constituents of the extracts, observe their effects and correlate them with the anti-inflammatory activity. Materials and methods: An infusion, a leaf rinse extract (LRE) and a polar extract from the rinsed leaves (PE) were obtained and analysed by HPLC-UV-DAD and infrared spectroscopy. The major compounds of these extracts were quantified. The three obtained extracts were evaluated for their anti-inflammatory activities using the paw oedema and croton oil ear oedema assays in mice. Furthermore, neutrophil migration was measured by evaluating myeloperoxidase activity. Results: The PE consists primarily of chlorogenic acids (CAs) and lacks sesquiterpene lactones (STLs). The LRE is rich in STLs and includes a few flavonoids. The infusion is chemically similar to the PE but also contains very low amounts of STLs. The PE and LRE have better mechanisms of action than non-steroidal anti-inflammatory drugs (NSAIDs). Unlike NSAIDs, both the PE and LRE inhibit oedema and neutrophil migration. The pool of CAs from the PE of T. diversifolia has an additional mechanism of action, and its anti-inflammatory effect was greater than what is described in the literature for this class of compounds using the same evaluation models. The similar chemical compositions observed for the infusion and the PE, contrasted with the different activities observed, suggests the presence of antagonist compounds produced during the extraction procedure (infusion); the infusion did not inhibit oedema, however it inhibited neutrophil migration. It suggests that although the great majority of plants present CAs, the category of anti-inflammatory effect of their extracts depends on a suitable pool of compounds and an absence of antagonists, among other factors. Conclusions: CAs from T. diversifolia comprise a good pool of anti-inflammatory compounds with better activity mechanisms than NSAIDs, other active compounds from the leaf extracts (STLs and flavonoids) and CAs from other plant sources. Thus, the PE of T. diversifolia has high potential for the development of new anti-inflammatory phytomedicines. The infusion probably contains antagonists, and therefore it can be useful to treat inflammation processes where neutrophil recruitment is involved and oedema is not. [Copyright &y& Elsevier]

Abstract: In the present study, an ultra performance liquid chromatography coupled with photo-diode array detector and time-of-flight mass spectrometry (UPLC–PDA–TOFMS) based chemical profiling approach to rapidly evaluate chemical consistency between traditional and dispensing granule decoctions of traditional medicine combinatorial formulae was proposed and validated using San–Huang–Xie–Xin–Tang (SHXXT) as a model combinatorial formula. Two different kinds of decoctions, namely traditional decoction: water extract of mixed three constituent herbs of SHXXT, and dispensing granules decoction: mixed water extract of each individual herbs of SHXXT, were prepared. Batches of these two kinds of decoction samples were subjected to UPLC–PDA–TOFMS analysis, the datasets of t R–m/z pairs, ion intensities and sample codes were processed with supervised orthogonal partial least squared discriminant analysis (OPLS–DA) to holistically compare the difference between these two kinds of decoction samples. Once a clear classification trend was found in score plot, further statistics was performed to generate S-plot, in which the variables (t R–m/z pair) contributing most to the difference were clearly depicted as points at the two ends of “S”, and the components that correlate to these ions were regarded as the most changed components during decocting of combinatorial formula. The identities of the changed components can be identified by comparing the mass/UV spectra and retention times with those of reference compounds and/or tentatively assigned by matching empirical molecular formulae with those of the known compounds published in the literatures. Using the proposed approach, global chemical difference was found between traditional and dispensing granule decoctions, and berberine, palmatine, epiberberine, baicalin, wonogoside, 2-O-golloyl-1-O-cinnamoylglucose and emodin were identified as the most changed components during decocting SHXXT. It is suggested that this newly established approach could be used practically for the evaluation of chemical consistency between traditional and dispensing granule decoctions of traditional medicine combinatorial formulae. [Copyright &y& Elsevier]

Justicia vahlii Roth. (Acanthaceae), also called as kodasoori and bhekkar is an annual therophyte erect or decumbent herb used traditionally in toothache, skin diseases (itching, topical inflammation) and for the treatment of various respiratory disorders. The current study aimed at exploring pain cessation potential of J. vahlii Roth. via murine model of neuropathic pain and its phytochemical, toxicological and antioxidant profiles. The hydro-alcoholic extract of J. vahlii (HAEJv) prepared by maceration technique was subjected to preliminary phytochemical screening, total bioactive content determination, UPLC-QTOF-MS and GC-MS analysis. Toxicity assessment was carried out by using brine shrimp lethality assay and acute oral toxicity test. Murine model of neuropathic pain was applied to assess the antineuropathic potential of the species. Furthermore effect of the extract on catalase, superoxide oxide dismutase (SOD), Glutathione (GSH), interleukin-1beta (IL-1β) and total necrosis factor-alpha (TNF-α) was also studied. In vitro antioxidant profile was explored by using four methods; 2,2-diphenyl-1-picrylhydrazyl (DPPH), 2,2-azinobis(3-ethylbenothiazoline)-6-sulfonic acid (ABTS), CUPric reducing antioxidant capacity (CUPRAC) and Ferric reducing antioxidant power (FRAP) assay. The phytochemical screening revealed the presence of phenols, flavonoids, coumarins, alkaloids and lignans as the major classes of secondary metabolites. The extract was found rich in total phenolics content (TPC) and total flavonoids content (TFC) with identification of total 59 bioactives in UPLC-QTOF-MS and 40 compounds in GC-MS analysis. The extract was found nontoxic up to 4000 mg/kg (p.o.) in mice and no mortality observed in brine shrimp lethality assay. The HAEJv significantly reduced number of acetic acid induced abdominal constrictions at 100 mg/kg (p < 0.01) and 200 mg/kg (p < 0.001) and increased paw withdrawal threshold p < 0.05 at 100 mg/kg and p < 0.001 at 200 mg/kg, and an increase in tail withdrawal latency time p < 0.001 at 200 mg/kg was observed. The extract significantly increased levels of catalase, SOD and GSH while decreased IL-1β and TNF-α levels in sciatic nerve tissue of mice. HAEJv showed highest antioxidant activity through CUPRAC method 121.32 ± 1.22 mg trolox equivalent per gram of dry extract (mg TE/g DE) followed by DPPH 81.334 ± 4.35 mg TE/g DE, FRAP 69.89 ± 3.05 mg TE/g DE and ABTS 38.17 ± 2.12 mg TE/g DE. The current study back the traditional use of J. vahlii in pain cessation through antioxidant based antineuropathic pain activity and revealed the extract non-toxic with number of functional phytoconstituents and warrants further research on isolation of the compounds and sub-acute toxicity studies. [Display omitted] • Justicia vahlii Roth. is traditionally used in South Asia for treating toothache and skin diseases. • Identification of bioactives in hydro-alcoholic extract was performed using UPLC-QTOF-MS and GC-MS analysis. • The brine shrimp lethality assay and acute oral toxicity confirmed the non-toxic nature of the extract. • The extract attenuated vincristine induced neuropathic pain, increased oxidative stress markers and decreased inflammatory mediators in mice. • Flavonoids may be the core phytoconstituents responsible for the pharmacological effects of the extract. [ABSTRACT FROM AUTHOR]

Pogostemon cablin Benth (PCB) is a well-known traditional Chinese medicine that has been used for treatment of many ailments for several centuries. In presently, the chemical profiling and quality control study of PCB has mainly concentrated on the volatile fractions. However, the non-volatile chemical profile of PCB was still unclear. In this study, 73 non-volatile constituents (i.e., 33 flavonoids, 21 organic acids, 9 phenylpropanoids, 4 sesquiterpenes, 3 alkaloids, and 3 other types of compounds) were identified and characterized in PCB using high performance liquid chromatography coupled with quadruple time-of-flight tandem mass spectrometry (HPLC-Q-TOF-MS). Meanwhile, to assess PCB samples, an established HPLC-Q-TOF-MS fingerprint was combined with multivariate statistical analysis that included similarity analysis (SA), hierarchical cluster analysis (HCA), principal component analysis (PCA), and orthogonal partial least squares-discriminant analysis (OPLS-DA). The PCB samples could be classified into two groups (herbal decoction pieces and processed medicinal materials), and acteoside, isoacteoside, 4′,6-Dihydroxy-5,7-dimethoxyflavone, pachypodol and pogostone were screened as the potential chemical markers that attributed classification. In addition, nine representative components (pachypodol, vicenin-2, apigenin, rhamnocitrin, acteoside, isoacteoside, chlorogenic acid, azelaic acid and pogostone) in PCB were simultaneously determined by using an ultra-high-performance liquid chromatography coupled with triple quadrupole tandem mass spectrometry (UPLC-QQQ-MS/MS). This study is the first to describe the chemical profile of PCB using liquid chromatography tandem mass spectrometry, which would improve our understanding of the substance basis of PCB and is helpful to the PCB further quality evaluation. [Display omitted] • The non-volatile chemical profile of Pogostemon cablin Benth (PCB) was revealed for the first time using HPLC-Q-TOF-MS. • An established HPLC-Q-TOF-MS fingerprint of PCB combined with the multivariate statistical analysis used to assess PCB samples. • A quick and sensitive UPLC-QQQ-MS/MS method was established and used to simultaneously quantify nine representative components in the PCB samples. • Five components were screened and identified as the potential chemical markers for the classification of herbal decoction pieces and processed medicinal materials of PCB. [ABSTRACT FROM AUTHOR]

Garden-cultivated Ginseng (GG) and mountain-cultivated Ginseng (MG) both belong to Panax Ginseng C. A. Meyer. However, the effective substances which can be used to distinguish GG from MG remain obscure. Therefore, the purpose of this study was to screen for discriminating markers that can assist in the correct identification of GG and MG. HPLC Q-TOF/MS and various chemometrics methods were used to analyze the chemical profiles of 13 batches of Ginseng and to explore the characteristic constituents of both GG and MG. The hepatocyte-protecting effects of GG and MG were investigated through a paclitaxel-induced liver injury model. Through a combination of correlation analysis and bioinformatic techniques, markers for differentiation between GG and MG were ascertained. A total of 40 and 41 compounds were identified in GG and MG, respectively, and 15 characteristic ingredients contributed significantly to the discrimination of GG from MG. Correlation analysis and network pharmacology were applied and ginsenosides Rg1, Re, Rb1, Rc, Rb2, and Rg3 were found to be discriminating markers of GG and MG. Six markers for the identification of GG and MG were screened out by a step-wise mutually oriented "chemical profiling–pharmaceutical effect" correlation strategy, which is of great significance for future quality assessment of Ginseng products. [ABSTRACT FROM AUTHOR]

Flavan-3-ols and proanthocyanidins of invasive alien plants Japanese knotweed (Fallopia japonica Houtt.), giant knotweed (Fallopia sachalinensis F. Schmidt) and Bohemian knotweed (Fallopia × bohemica (Chrtek & Chrtkova) J.P. Bailey) were investigated using high performance thin-layer chromatography (HPTLC) coupled to densitometry, image analysis and mass spectrometry (HPTLC–MS/MS). (+)-Catechin, (−)-epicatechin, (−)-epicatechin gallate and procyanidin B2 were found in rhizomes of these three species, and for the first time in Bohemian knotweed. (−)-Epicatechin gallate, procyanidin B1, procyanidin B2 and procyanidin C1 were found in giant knotweed rhizomes for the first time. Rhizomes of Bohemian and giant knotweed have the same chemical profiles of proanthocyanidins with respect to the degree of polymerization and with respect to gallates. Japanese and Bohemian knotweed have equal chromatographic fingerprint profiles with the additional peak not present in giant knotweed. Within the individual species giant knotweed rhizomes and leaves have the most similar fingerprints, while the fingerprints of Japanese and Bohemian knotweed rhizomes have additional peaks not found in leaves. Rhizomes of all three species proved to be a rich source of proanthocyanidins, with the highest content in Japanese and the lowest in Bohemian knotweed (based on the total peak areas). The contents of monomers in Japanese, Bohemian and giant knotweed rhizomes were 2.99 kg/t of dry mass (DM), 1.52 kg/t DM, 2.36 kg/t DM, respectively, while the contents of dimers were 2.81 kg/t DM, 1.09 kg/t DM, 2.17 kg/t DM, respectively. All B-type proanthocyanidins from monomers to decamers (monomers—flavan-3-ols, dimers, trimers, tetramers, pentamers, hexamers, heptamers, octamers, nonamers and decamers) and some of their gallates (monomer gallates, dimer gallates, dimer digallates, trimer gallates, tetramer gallates, pentamer gallates and hexamer gallates) were identified in rhizomes of Bohemian knotweed and giant knotweed. Pentamer gallates, hexamers, hexamer gallates, nonamers and decamers were identified for the first time in this study in Bohemian and giant knotweed rhizomes. [ABSTRACT FROM AUTHOR]

• Chemical profiling and network pharmacology-based analysis of JWQFY were performed. • A total of 135 constituents were identified, 70 of them were further quantified. • Multi-target mechanisms of JWQFY against Alzheimer's disease were predicted. • The modification rationality of the formula JWQFY was elucidated. Jia-Wei-Qi-Fu-Yin (JWQFY) is a newly developed anti-Alzheimer's disease (AD) prescription modified from a classical traditional Chinese medicine formula, Qi-Fu-Yin (QFY). However, a systematic understanding of its chemical constituents and molecular mechanisms is still elusive. To address this problem, comprehensive chemical profiling followed by network pharmacology-based analysis of JWQFY was performed. Firstly, a total of 136 compounds were characterized by high performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (HPLC-QTOF MS), 17 of them were specifically identified in JWQFY comparing with QFY. Seventy compounds were further quantified via a validated HPLC coupled with triple quadrupole tandem mass spectrometry (QQQ MS) method. Then the protein targets of the seventy compounds were gathered from public databases for network construction. As a result, fifty-seven compounds were filtered, which interacted with 655 targets. Thirty-four of them were mapped into the KEGG pathway of AD, indicating JWQFY might exert anti-AD effects by anti-inflammation, neuronal apoptosis intervening, Aβ production inhibition and phosphorylating tau protein moderating. Furthermore, in the compound-target-AD network, a list of hub compounds and hub targets was identified based on their topological features, including the degree, node betweenness and closeness. Four of the hub compounds were specifically originated from JWQFY, supporting the modification rationality of this formula. This study provided a scientific basis for understanding the bioactive compounds and the multi-target mechanism of JWQFY. [ABSTRACT FROM AUTHOR]

Semiliquidambar cathayensis Chang was a traditional medicinal plant and used to treat rheumatism arthritis and rheumatic arthritis for centuries in China with no scientific validation, while only 15 components were reported. Thus, a rapid, efficient, and precise method based on ultra-high-performance liquid chromatography coupled with quadrupole time-of-flight tandem mass spectrometry (UHPLC-Q-TOF-MS/MS) was applied in both positive- and negative-ion modes to rapidly analysis the main chemical compositions in S. cathayensis for the first time. Finally, a total of 85 chemical compositions, including 35 alkaloids, 12 flavonoids, 7 terpenoids, 5 phenylpropanoids, 9 fatty acids, 7 cyclic peptides, and 10 others were identified or tentatively characterized in the roots of S. cathayensis based on the accurate mass within 5 ppm error. Moreover, alkaloid, flavonoid, phenylpropanoid, and cyclic peptide were reported from S. cathayensis for the first time. This rapid and sensitive method was highly useful to comprehend the chemical compositions and will provide scientific basis for further study on the material basis, mechanism and clinical application of S. cathayensis roots. [ABSTRACT FROM AUTHOR]

Monascus -fermented rice product (MFRP) has been regarded as a dietary supplement and traditional medicine with circulation-promoting effects in China and other countries for centuries. This study was carried out to profile the chemical components in MFRP, and provide available information for elucidating the potential lipid-lowering compounds other than monacolins. High-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-QTOF MS) and gas chromatography coupled with mass spectrometry (GC-MS) methods were applied to comprehensive analysis of chemical components in MFRP. Potential small molecules were identified by comparing with reference standards, or tentatively characterized by comparing their retention time and high-resolution mass spectral data with previous literature. The lipid-lowering properties of ten major non-monacolin compounds were evaluated in cholesterol-fed zebrafish larvae. And one with optimum lipid-lowering activity was subsequently evaluated in high fat diet-fed C57BL/6 J mice, with the dyslipidemia and ectopic lipid deposition being investigated. A total of 99 compounds were characterized in MFRP, including 38 monacolins, 5 decalins, 6 isoflavones, 13 pigments, 8 azaphilonoids, 11 amino acids, 4 nucleosides, 9 lipid acids, 4 phytosterols and glycerol. The preliminary screening showed that ergosterol remarkably reduced cholesterol levels in zebrafish larvae. Moreover, ergosterol delayed body weight gain and decreased circulating total cholesterol, triglyceride, low density lipoprotein cholesterol levels in high fat diet-fed mice. Ectopic lipid accumulation was also ameliorated in the liver and heart of obese mice. Global analysis of chemical components and screening of lipid-lowering non-monacolin compounds in MFRP have improved our understanding of its therapeutic material basis. Image 1 [ABSTRACT FROM AUTHOR]

Lobelia chinensis is a kind of herbal medicine widely distributed and used in Asia. The chemical components of this herb, however, have not been well studied until now. Lobeline, as an essential and famous bioactive compound in Lobelia genus, has been assumed to be present in L. chinensis. In order to ascertain its presence and, more importantly, proper use of this herb, chemical profiling this herb with highly sensitive and high-resolution analytical mass spectrometry was applied. In this study, high-performance liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC/Q-TOF MS) method was employed to systematically profile the chemical constituents of L. chinensis for the first time. Comparative chemical profiling study of L. chinensis and Lobelia inflata was also conducted to provide evidence whether lobeline is present or not. Piperidine alkaloids except for lobeline, alkaloid-lignan hybrids, flavonoids, polyacetylenes, nonanedioic acid, and some new phytochemicals were successfully identified in L. chinensis simultaneously. Comparing to the chemical profiles of L. inflata, lobeline was found to be absent in L. chinensis. All of the secondary metabolites in L. chinensis were determined with the HPLC/Q-TOF MS method. The absence of lobeline in L. chinensis was confirmed after this extensive study. [ABSTRACT FROM AUTHOR]