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Abstract: Radix Polygoni Multiflori, Rhizoma et Radix Polygoni Cuspidati, and Radix et Rhizoma Rhei are the most frequently used traditional Chinese medicines in the family Polygonaceae. The three herbal medicines (HMs) contain similar types of compounds. In Chinese Pharmacopoeia, five high-performance liquid chromatography (HPLC) coupled with ultraviolet (UV) detection methods have been employed for their quality control. The aim of this study was to develop a simple and conventional strategy, segmental monitoring based on variable wavelength detection (VWD), for simultaneous quantification of phenolic acids, flavonoids, stilbenes and anthraquinones in the three chemically analogous HMs. Compared with the commonly used HPLC-diode array detection (DAD), the proposed method afforded desirable performance on linearity, precision and sensitivity. Additionally, a quadrupole time-of-flight mass spectrometry (QTOF-MS) was applied to the structural confirmation of analytes from complex matrices. Based on the chemical profiles and contents of the analyses, 27 samples from three HMs were well classified using the principal component analysis. The results of this study demonstrated the potential and applicability of segmental monitoring strategy based on VWD for comprehensive quality control of HMs. [Copyright &y& Elsevier]

Abstract: In this work, the metabolite profiles of Danggui Buxue Tang (DBT) in rat bile and plasma were qualitatively described, and the possible metabolic pathways of DBT were subsequently proposed. Emphasis was put on correlative analysis of metabolite profiling in different biological fluids. After oral administration of DBT, bile and plasma samples were collected and pretreated by solid phase extraction. Rapid resolution liquid chromatography coupled to time-of-flight mass spectrometry (RRLC–TOFMS) was used for characterization of DBT-related compounds (parent compounds and metabolites) in biological matrices. A total of 142 metabolites were detected and tentatively identified from the drug-containing bile and plasma samples. Metabolite profiling shows that rat bile contained relatively more glutathione-derived conjugates, more saponins compounds and more diverse forms of metabolites than urine. The metabolite profile in plasma revealed that glucuronide conjugates of isoflavonoids, dimmers, acetylcysteine conjugates and parent form of phthalides, as well as saponin aglycones were the major circulating forms of DBT. Collectively, the metabolite profile analysis of DBT in different biological matrices provided a comprehensive understanding of the in vivo metabolic fates of constituents in DBT. [Copyright &y& Elsevier]

Abstract: The fact that the effects of herbal medicines (HMs) are brought about by their chemical constituents has created a critical demand for powerful analytical tools performing the chemical analysis to assure their efficacy, safety and quality. Liquid chromatography coupled to mass spectrometry (LC–MS) is an excellent technique to analyze multi-components in complex herbal matrices. Due to its inherent characteristics of accurate mass measurements and high resolution, time-of-flight (TOF) MS is well-suited to this field, especially for qualitative applications. The purpose of this article is to provide an overview on the potential of TOF, including the hybrid quadrupole- and ion trap-TOF (QTOF and IT-TOF), hyphenated to LC for chemical analysis in HMs or HM-treated biological samples. The peculiarities of LC–(Q/IT)TOF-MS for the analysis of HMs are discussed first, including applied stationary phase, mobile-phase selection, accurate mass measurements, fragmentation and selectivity. The final section is devoted to describing the applicability of LC–(Q/IT)TOF-MS to routine analysis of multi-components, including target and non-target (unknown) compounds, in herbal samples, emphasizing both the advantages and limitations of this approach for qualitative and quantitative purposes. The potential and future trends of fast high-performance liquid chromatography (HPLC) (e.g. rapid resolution LC and ultra-performance LC) coupled to (Q)TOF-MS for chemical analysis of HMs are highlighted. [Copyright &y& Elsevier]

A quantitative HPLC-MS method was developed for rapid and sensitive analysis of 5 tannins (gallotannins and proanthocyanidin types) and 5 monoterpene glycosides (pinane type) in 70% ethanol extract of Radix Paeoniae Alba (RPA). The total analysis time was less than 10 minutes without a loss in resolution using a short column packed with 1.8 µm porous particles, six times faster than the performance of conventional columns of 5.0 µm porous particles. This assay was fully validated with respect to precision, repeatability, and accuracy. All calibration curves showed good linear regression (r2 > 0.9961), and recoveries of all analytes fell in the ranges of 92.0-104.1%. The developed method was successfully applied to analysis of the 10 marker compounds in 6 processed RPA products and 27 commercial samples from different pharmacies in China. The quantitative results demonstrated that samples processed in different ways and from different provinces showed varied qualities based on the contents of active components. Robustness and applicability of the method offered a rapid, sensitive, and validated method for routine analysis and quality control of this herbal medicine. Meanwhile, the LC/MS method developed here provided a more economical alternative for laboratories looking into improving separation and increasing throughput, without the need to upgrade the existing HPLC system to a special ultra fast HPLC system. [ABSTRACT FROM AUTHOR]

Abstract: A dynamic microdialysis sampling method with liquid chromatography–diode array detection and time-of-flight mass spectrometry (LC–DAD–TOF/MS) analysis was developed to investigate rat microsomal metabolisms of calycosin and formononetin, and their drug–drug interactions. Two hydroxylated metabolites from calycosin, and three hydroxylated or 4′-O-demethylated derivatives from formononetin were detected and identified after co-incubation with microsomes. Calibration curves offered linear ranges of two orders of magnitude with r 2 >0.999 for calycosin, formononetin and daidzein. The quantitative LC method provides a range of 0.028–0.034μg/mL for limits of detection, overall precision less than 5% and accuracy less than 3% by RSD. Besides, calycosin and formononetin were found to produce the depressive effect on the CYP450 enzyme reaction, and inhibit phase I enzyme reaction of each other when they are concurrent. Dynamic microdialysis sampling with LC–DAD–TOF/MS analysis developed in this work is a powerful tool for in vitro metabolism studies of drugs and metabolic interactions. [Copyright &y& Elsevier]

Abstract: A high-performance liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry (HPLC–ESI-TOF-MS) method has been developed for qualitative and quantitative analysis of isoflavonoids and saponins, as well as for the quality control of Radix Astragali and its preparations. The selectivity, reproducibility and sensitivity are compared with HPLC with diode array detection (DAD) and evaporative light scattering detection (ELSD). Limits of detection and quantification fell in ranges of 9–40 and 23–103ng/mL for 13 analytes with a injection of 10μL samples, and all calibration curves showed good linear regression (r 2 >0.9938) within the test range. The assay was successfully utilized to analyze the 13 marker components in 20 samples of Radix Astragali products. The quantitative results demonstrated that samples from different localities and manufacturers showed different quality. Advantages, in comparison with conventional HPLC–DAD–ELSD, are that reliable identification of target compounds could be achieved by accurate mass measurements (<3ppm) along with characteristic retention time, extracted ions chromatograms using a narrow mass window for quantification ensure that the chromatographic peaks are free from background or co-elutes interference, and the great enhancement in selectivity and sensitivity allows identification and quantification of low levels of constituents in complex Radix Astragali matrixes. [Copyright &y& Elsevier]

Abstract: A quantitative method by ultra-fast HPLC coupled with time-of-flight mass spectrometry (TOF/MS) has been developed for analysis of 15 major constituents in Danggui Buxue Tang (DBT) preparations. Its performance was compared with a conventional HPLC method with diode array detection/evaporative light scattering detection (DAD/ESLD). Accurate mass measurements within 3ppm error were obtained for all the compounds. The analytical time by an ultra-fast system is 4 times faster than conventional HPLC, the limits of detection by TOF/MS are low to 0.004–0.08ng compared with 1–200ng for HPLC–DAD–ELSD, and acceptable linearity of response was demonstrated over two orders of magnitude (r 2 >0.99) for all analytes. Intra-day reproducibility was below 3% and inter-day values were below 5% R.S.D. Robustness and applicability of the method was validated for the analysis of market DBT real samples, proposing a rapid, sensitive and validated method for routine analysis and quality control of DBT. [Copyright &y& Elsevier]

Abstract: A novel fast high-performance liquid chromatography (HPLC) method coupled with diode array detection (DAD) and time-of-flight mass spectrometry (TOF/MS) was developed for qualitative and quantitative analysis of Radix Astragali products. The potential of fast HPLC on 1.8-μm particles was compared with the performance of HPLC on conventional 5-μm particles columns. Significant advantages of fast HPLC include high-speed chromatographic separation, four times faster than HPLC with conventional columns, and great enhancement in sensitivity with limits of detection low to 0.001ng. With dynamic adjustment of fragmentor voltage in TOF/MS, an efficient transmission of the ions was achieved to obtain the best sensitivity and abundant fragmentation. By accurate mass measurements within 5ppm error for each molecular ion and subsequent fragment ions, a reliable identification and differentiation of six major saponins including two groups of isomers and twelve main isoflavonoids was described here for the first time. For quantitative analysis by fast HPLC–TOF/MS, linearity of response over two orders of magnitude was demonstrated (r 2 >0.99) for all analytes. Intra-day reproducibility was below 3% RSD and inter-day values were below 5% RSD. A good correlation (slope=1.1108, r 2 =0.9853) was observed for accuracy test. It is concluded that the fast and sensitive HPLC-DAD–TOF/MS is powerful in qualitative and quantitative analysis of complex herbal medicines in terms of time savings, sensitivity, selectivity, precision, accuracy as well as increasing sample throughout and lowering solvent consumption. [Copyright &y& Elsevier]

Abstract: A method, high-performance liquid chromatography coupled with diode array and evaporative light scattering detectors (HPLC-DAD-ELSD), was developed to evaluate the quality of Radix Astragali through a simultaneous determination of six major active isoflavonoids and four main saponins. The wavelength at 280nm was chosen to determine six isoflavonoids: calycosin-7-O-β-d-glucoside (1), ononin (2), (6αR, 11αR)-9,10-dimethoxypterocarpan-3-O-β-d-glucoside (3), (3R)-2′-hydroxy-3′,4′-dimethoxyisoflavan-7-O-β-d-glucoside (4), calycosin (5), and formononetin (6); and ELSD connected after DAD was employed to determine four saponins: astragaloside IV (7), astragaloside II (8), astragaloside I (9), and acetylastragaloside I (10). This assay was fully validated with respect to precision, repeatability and accuracy. The proposed method was successfully applied to quantify the ten components in eleven samples from different localities in China; significant variations were demonstrated in the content of these compounds in the samples from different areas. This simple, rapid, low-cost and reliable HPLC-DAD-ELSD method is suitable for routine quantitative analysis and quality control of traditional Chinese medicines (TCMs) consisting of bioactive multi-components with different structures such as Radix Astragali. [Copyright &y& Elsevier]

Abstract: Belamcandae Rhizoma, derived from the rhizome of Belamcanda chinensis (L.) DC., has been used as traditional Chinese medicine for the treatment of coughing and pharyngitis. However, there have been few studies dealing with the systematic analysis of the bioactive constituents in Belamcandae Rhizoma. In this work, high performance liquid chromatography–diode array detection–electrospray ionization multiple-stage mass spectrometry (HPLC-DAD-ESI-MS n ) combined with liquid chromatography–time of flight-mass spectrometry (HPLC–TOF/MS) was established for profiling and characterization of multi-constituent in Belamcandae Rhizoma. The ESI-MS n fragmentation behaviors of the authentic references were proposed for aiding the structural identification of components in the extract. Thirty-five flavonoids, including 30 isoflavones and five xanthones, were identified or tentatively identified by comparing their retention times, UV and MS spectra with those of authentic compounds or literature data. Twelve of the identified compounds (neomangiferin, mangiferin, tectoridin, iristectorin B, iristectorin A, iridin, tectorigenin, iristectorigenin A, irigenin, irisflorentin, irilone and dichtomitin) were determined by HPLC–DAD using a C18 column. The results indicated that the developed analysis method could be employed as a rapid, effective technique for structural characterization of chemical constituents in herbal medicine. This work is expected to provide comprehensive information for the quality evaluation of Belamcandae Rhizoma, which would be a valuable reference for the further study and development of this herb and related medicinal products. [Copyright &y& Elsevier]

Ethnopharmacological relevance: Devil''s Club (Oplopanax horridus) is one of the most important spiritual and medicinal plants to many indigenous peoples of Alaska and the Pacific Northwest. It is widely used for external and internal infections as well as arthritis, respiratory ailments, digestive tract ailments, broken bones, fever, headaches, and cancer. Aim of the study: To investigate hydrophobic constituents and their potential anticancer activity from Devil''s Club, Oplopanax horridus. Materials and methods: The root bark extract of Oplopanax horridus was isolated by chromatographic techniques. Structures of isolated compounds were identified by spectroscopic methods and comparison with published data. The anti-proliferation of isolated hydrophobic constituents in human breast cancer MCF-7 cells, human colon cancer SW-480 and HCT-116 cells were tested. The potential mechanism of anti-proliferation was also investigated using cell cycle and apoptosis assays. Results and discussion: Six compounds were isolated and structurally identified as 9,17-octadecadiene-12,14-diyne-1,11,16-triol, 1-acetate (1), oplopandiol acetate (2), falcarindiol (3), oplopandiol (4), trans-nerolidol (5) and t-cadinol (6). These compounds showed potential anticancer activities on human breast cancer and colon cancer cells, of which compound 3 possesses the strongest activity. Further cell cycle and apoptosis tests by flow cytometry showed the polyacetylenes 1–4 induced HCT-116 cell arresting in G2/M phase and inhibited proliferation by the induction of apoptosis at both earlier and later stages. Conclusion: These results provide promising baseline information for the potential use of Oplopanax horridus, as well as some of the isolated compounds in the treatment of cancer. [Copyright &y& Elsevier]

Abstract: A method based on the on-line turbulent-flow chromatography and fast high-performance liquid chromatography/mass spectrometry (TFC–LC/MS) was developed for sensitive and high throughput pharmacokinetic study of traditional Chinese medicines (TCMs). In this method, an on-line extraction column (Waters Oasis HLB) and a fast HPLC column with sub-2μm particle size (Agilent Zorbax StableBond-C18, 4.6mm×50mm, 1.8μm) in a column-switching set-up were utilized. HLB is a reversed-phase extraction column with hydrophilic–lipophilic balanced copolymer (2.1mm×20mm, 25μm particle size), which will exhibit some turbulent-flow properties at a high-flow rate. The method combines the speed and robustness of turbulent-flow extraction and the sensitivity and separation efficiency of fast HPLC–MS to analyze multiple and trace constituents of TCMs in plasma matrix. This method was successfully applied for pharmacokinetic study of verticine, verticinone and isoverticine, the chemical markers of Fritillaria thunbergii, after oral administration of total steroidal alkaloids extract of F. thunbergii to rats. Each plasma sample was analyzed within 7min. The method demonstrated good linearity (R >0.999) ranged from 0.505 to 96.0ng/mL with satisfactory accuracy and precision, and the lower limit of quantifications of verticine, verticinone and isoverticine were estimated to be 0.120, 0.595 and 0.505ng/mL, respectively. These results indicate that the proposed method is fast, sensitive, and feasible for pharmacokinetic study of TCMs. [Copyright &y& Elsevier]

Abstract: Harpagoside, a major bioactive iridoid glucoside in genus Scrophularia, has been widely used in clinical practice for the treatment of pain in the joints and lower back for its neuroprotective and anti-inflammation activities. To investigate the pharmacokinetics and hepatobiliary excretion, an in vivo microdialysis method coupled with high performance liquid chromatography was developed to monitor the concentration of harpagoside in blood and bile. The harpagoside bile-to-blood distribution ratio (AUC bile/AUC blood) up to 986.28±78.46 significantly decreased to 6.41±0.56 or 221.20±18.92 after co-administration of cyclosporin A or verapamil. The results indicated that harpagoside went through concentrative elimination from the bile which was probably regulated by P-glucoprotein, providing possible clinical trials of co-administration of transporter inhibitors to decrease drug efflux, thus to enhance the curative effects. [Copyright &y& Elsevier]

This work aimed to establish a systematic strategy to enrich and separate quercetin-3- O -β- d -glucuronide (Q3GA) from lotus leaves with macroporous resin and semi-preparative HPLC. Six resins were tested, and LX-5 was chosen as the appropriate resin for Q3GA based on the adsorption and desorption performances. After one-step enrichment, the content of Q3GA increased from 2.15% in crude extract to 52.25% in 30% ethanol fraction with yield of 11.97%. The Q3GA was then isolated from the 30% ethanol fraction by semi-preparative HPLC, and the purity of Q3GA was above 98.00% with yield of 19.76%. These results suggested that the aforementioned strategy was a useful and economic method to enrich and separate Q3GA from lotus leaves. Additionally, the anti-inflammatory effect of Q3GA was evaluated in lipopolysaccharide-treated RAW264.7 macrophages, and the result demonstrated that Q3GA could significantly inhibit LPS-induced NO release in vitro in a dose-dependent manner compared with control group. [ABSTRACT FROM AUTHOR]

Most Aconitum species, also known as aconite, are extremely poisonous, so it must be identified carefully. Differentiation of Aconitum species is challenging because of their similar appearance and chemical components. In this study, a universal strategy to discover chemical markers was developed for effective authentication of three commonly used aconite roots. The major procedures include: (1) chemical profiling and structural assignment of herbs by liquid chromatography with mass spectrometry (LC-MS), (2) quantification of major components by LC-MS, (3) probabilistic neural network (PNN) model to calculate contributions of components toward species classification, (4) discovery of minimized number of chemical markers for quality control. The MS fragmentation pathways of diester-, monoester-, and alkyloyamine-diterpenoid alkaloids were compared. Using these rules, 42 aconite alkaloids were identified in aconite roots. Subsequently, 11 characteristic compounds were quantified. A component–species modeling by PNN was then established combining the 11 analytes and 26-batch samples from three aconite species. The contribution of each analyte to species classification was calculated. Selection of fuziline, benzoylhypaconine, and talatizamine, or a combination of more compounds based on a contribution order, can be used for successful categorization of the three aconite species. Collectively, the proposed strategy is beneficial to selection of rational chemical markers for the species classification and quality control of herbal medicines. [ABSTRACT FROM AUTHOR]

Highlights: [•] A MSPD method for extraction and clean-up of ginkgo components. [•] UHPLC–QQQ-MS for simultaneous analysis of 18 ginkgo components. [•] Direct quantification of 10 flavonol glycosides without hydrolysis. [•] Analysis of the 12 Ginkgo biloba tablets available in the global market. [Copyright &y& Elsevier]

Highlights: [•] A universal HRPF strategy was developed for discovery of bioactive compounds. [•] This strategy realized high-purity peak fraction preparation in one HPLC run. [•] HRPF combined with a luciferase reporter gene assay to screen Nrf2 activators. [•] 20 diterpene quinones were screened out and unambiguously identified. [•] 16 compounds were reported to possess novel Nrf2 activation effect. [Copyright &y& Elsevier]

Abstract: In this study, an efficient strategy based on bioassay-guided fractionation, high-performance liquid chromatography/electrospray ionization quadrupole time-of-flight mass spectrometry (HPLC-ESI-Q/TOF-MS) and high-speed counter-current chromatography (HSCCC) was established to screen and purify bioactive compounds from Chinese herbal medicines (CHMs). This screening system was efficient and successfully applied to reveal anti-prostate cancer candidates from Puerariae thomsonii Flos. As a result, an active fraction with strong in vitro anti-prostate cancer activity was obtained, and the main compounds in the fraction were purified by HSCCC, giving 82mg of tectoridin, 36mg of tectorigenin-7-O-[β-d-xylopyranosyl-(1→6)-β-d-glucopyranoside and 64mg of tectorigenin. Among them, tectorigenin, possessing the highest anti-prostate cancer activity with IC50 value of 0.08μM, has priority to be lead compound. The results of this work demonstrated that the developed method was efficient and could be employed for the rapid screening, identification and purification of active components from CHMs. [Copyright &y& Elsevier]

Abstract: Various analytical technologies have been developed for quantitative determination of marker compounds in herbal medicines (HMs). One important issue is matrix effects that must be addressed in method validation for different detections. Unlike biological fluids, blank matrix samples for calibration are usually unavailable for HMs. In this work, practical approaches for minimizing matrix effects in HMs analysis were proposed. The matrix effects in quantitative analysis of five saponins from Panax notoginseng were assessed using high-performance liquid chromatography (HPLC). Matrix components were found to interfere with the ionization of target analytes when mass spectrometry (MS) detection were employed. To compensate the matrix signal suppression/enhancement, two matrix-matched methods, standard addition method with the target-knockout extract and standard superposition method with a HM extract were developed and tested in this work. The results showed that the standard superposition method is simple and practical for overcoming matrix effects for quantitative analysis of HMs. Moreover, the interference components were observed to interfere with light scattering of target analytes when evaporative light scattering detection (ELSD) was utilized for quantitative analysis of HMs but was not indicated when Ultraviolet detection (UV) were employed. Thus, the issue of interference effects should be addressed and minimized for quantitative HPLC–ELSD and HPLC–MS methodologies for quality control of HMs. [Copyright &y& Elsevier]

Abstract: Ginger, from the rhizome of Zingiber officinale Rosco (Zingiberaceae), is a common condiment for foods and beverages. In this work, we tested a hypothesis that a steaming process affects the chemical profile and anticancer potential of ginger. An HPLC method with TOF/MS and DAD was developed to analyse the chemical constituents in ginger. The antiproliferative effect of fresh, dried and steamed gingers was evaluated using human Hela cancer cells. The results showed that the antiproliferative effect of steamed ginger at 120°C for 4h was approximately 1.5- and 2-fold higher than that of dried and fresh ginger, respectively. Twenty-two components were characterised in the steamed ginger. The decreased concentration of gingerols and increased levels of shogaols contributed to the improved anticancer potential of the steamed ginger. This study elucidated the relationship of the heating process with the constituents and anticancer activity, and developed an optimised processed ginger extract for chemoprevention. [Copyright &y& Elsevier]

Abstract: A rapid high-performance liquid chromatography–mass spectrometry (HPLC–MS) method was developed and validated for simultaneous quantification of 6-gingerol, 8-gingerol, 10-gingerol and 6-shogaol in rat plasma after oral administration of ginger oleoresin. Plasma samples extracted with a liquid–liquid extraction procedure were separated on an Agilent Zorbax StableBond-C18 column (4.6mm×50mm, 1.8μm) and detected by MS with electrospray ionization interface in positive selective ion monitoring (SIM) mode. Calibration curves (1/x 2 weighted) offered satisfactory linearity (r 2 >0.995) in a wide linear range (0.0104–13.0μg/mL for 6-gingerol, 0.00357–4.46μg/mL for 8-gingerol, 0.00920–11.5μg/mL for 10-gingerol and 0.00738–9.22μg/mL for 6-shogaol). The lower limit of quantification (LLOQ) was in a range of 3.57–10.4ng/mL. The analytes and internal standard can be baseline separated within 6min. Inter- and intra-day assay variation was less than 15%. This developed method was successfully applied to pharmacokinetic studies of ginger oleoresin after oral administration to rats. Glucuronide of 6-gingerol was determined after β-glucuronidase hydrolysis for more information, and the intestinal glucuronidation was further confirmed by comparison of plasma samples of hepatic portal vein and femoral vein. [Copyright &y& Elsevier]

Abstract: Flos Lonicerae, referred to the flower buds of several medicinal Lonicera species, is a commonly used traditional Chinese herbal medicine. A multi-component-assay quality control method, using high performance liquid chromatography coupled with electrospray ionization time-of-flight mass spectrometry (HPLC-ESI/TOF MS), has been developed for the simultaneous identification and quantification of 32 bioactive compounds in Flos Lonicerae. The limits of detection (LOD) and quantification (LOQ) were in the range of 0.002–0.089 and 0.006–0.355μg/ml, respectively. All calibration curves showed good linear regression (r 2 ≥0.99) within the test ranges. The overall intra- and inter-day precisions of analytes were less than 3.47% for peak area and 0.38% for retention time. The recoveries were from 85.4% to 101.6%. The validated method was applied to assay of 32 compounds in 8 medicinal Lonicera species. Furthermore, six unknown chromatographic peaks were tentatively characterized. It was demonstrated that the HPLC-ESI/TOF MS method was suitable for quality control of Lonicera species, owing to the advantages of accurate mass analysis, resolving power, enhanced selectivity and high sensitivity. [Copyright &y& Elsevier]

Abstract: A novel strategy for predicting bioactive components in traditional Chinese medicines (TCM) using live cell extraction and high performance liquid chromatography–diode array detection–mass spectrometry (HPLC–DAD–MS) analysis was proposed. The hypothesis is that when cells are incubated together with the extract of TCM, the potential bioactive components in the TCM should selectively combine with the cells, and the relative concentrations of the cell-combining components in the suspension medium should decrease, while the cell-combining components would be detectable in the extract of denatured cells. The identities of the cell-combining components could be determined by HPLC–DAD–MS analysis. Using the proposed approach, the potential bioactive components of Danggui Buxue decoction, a commonly used TCM for anaemia, and its compositions, Radix Angelica Sinensis and Radix Astragli for endothelial cells, were investigated. Six compounds in the extract of Danggui Buxue decoction were detected as the components selectively combined with endothelial cells, among them two were contributed by Radix Angelica Sinensis, and four by Radix Astragli. The identities of four of the six potential bioactive compounds were elucidated as ononoside, calycosin, 3-butylphthalide and ligustilide by HPLC–DAD–MS analysis. The results indicate that the proposed approach may be applied to predict the bioactive candidates in TCM. [Copyright &y& Elsevier]

• Nephrotoxic aristolochic acids was analyzed with gold nanoclusters for the first time. • The detection can be finished within 30 s. • This method can be applied to biological samples and phytomedicines extracts. • A portable fluorescent test papers was developed for AAs-containing plants detection. Aristolochic acids (AAs), the main compounds of Aristolochia plants, have aroused increasing attention due to their irreversible nephrotoxicity, carcinogenicity and mutagenicity. Common approaches for AAs monitoring usually need expensive equipment, specially trained manipulators and time-consuming procedures. Thus, it is desirable to develop a simple, fast and easy to use approach for AAs detection. Herein, we reported a fluorescent approach to detect AAs by using the lysozyme-functionalized Au nanoclusters (Lys-AuNCs) as probe. The probe shows excellent tolerance to environment temperature and pH, and it is proved to work successfully for AAs detection in real samples (serum, plasma, urine and herbal extracts). Compared with high-performance liquid chromatography method (HPLC), fluorescence method can be finished within 1 min with a recovery of 117.49 %. With the help of the visible fluorescence as signal, a paper sensor is further prepared for a direct visual monitoring of AAs. It also exhibits good stability in various conditions. After the addition of AA-I, a concentration-dependent fluorescence signal on paper was observed by naked eyes under a UV lamp. The developed paper-based fluorescent sensor provides a portable and simple method for AAs detection in herbal products and environment. [ABSTRACT FROM AUTHOR]

As a classic herbal prescription, Huanglian Jiedu Decoction (HLJDD) exhibits positive effects against cardiac dysfunction. However, its cardioprotective effects and potential mechanism(s) of action still need to be systematically investigated. This study aimed to reveal the underlying therapeutic mechanism of HLJDD on transverse aortic constriction (TAC)-induced pathological cardiac hypertrophy and remodeling. TAC-induced cardiac hypertrophy and remodeling mice model was established to evaluate the therapeutic effects of HLJDD. Serum untargeted metabolomics and lipidomic profiling were performed using ultra-performance liquid chromatography quadrupole-time-of-flight mass spectrometry coupled with multivariate statistical analyses. Oral administration of HLJDD (2.5 g/kg/day, 5.0 g/kg/day) significantly improved the heart morphology, enhanced the heart function, and alleviated the accumulation of fibrosis in the interstitial space and the infiltration of inflammatory cells in TAC-stimulated mice. Serum untargeted metabolomics analysis showed that significant alterations were observed in metabolic signatures between the TAC-model and sham group. Principal component analysis and orthogonal partial least-squares discriminant analysis screened 59 differential metabolic features and 13 metabolites were identified. The disturbed metabolic pathways in TAC group mainly related to lipid metabolism. Further serum lipidomic profiling showed that most lipids including cholesterol esters, ceramides, glycerides, fatty acids and phospholipids were decreased in TAC group and these alterations were reversed after HLJDD intervention. HLJDD alleviates TAC-induced pathological cardiac hypertrophy and remodeling, and its potential therapeutic mechanism involves the regulation of lipid metabolism. Image 1 [ABSTRACT FROM AUTHOR]