Combining HPLC-DAD-QTOF-MS and HPLC-SPE-NMR to Monitor In Vitro Vitetrifolin D Phase I and II Metabolism.
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ABSTRACT:
SUBMITTER: Sturm S
PROVIDER: S-EPMC8400717 | biostudies-literature |
REPOSITORIES: biostudies-literature
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Project description:Kaixin Powder (KXP) is a classic formula for treating morbid forgetfulness in ancient China. To guarantee the efficacy and safety of KXP, a simple and accurate HPLC-DAD method has been established and validated for the quantitative analysis of seven bioactive compounds in KXP. Dehydrotumulosic acid (DTU) and dehydrotrametenolic acid (DTR) were quantified in KXP for the first time. Good chromatographic separation was conducted on a Kromasil 100-5 C18 column (250 mm × 4.6 mm, 5 μm) by gradient elution using mobile phases containing acetonitrile and 0.1% formic acid aqueous solution at different detection wavelengths. The calibration curves of each compound showed good linearity (r ≥ 0.9990), and the LOD and LOQ were in the ranges of 0.01-0.10 and 0.03-0.40 μg/mL, respectively. The relative standard deviations (RSDs) of intra-day and inter-day precisions were in the ranges of 0.45-1.74% and 0.56-2.32%, respectively. All recoveries were in the range of 93.6-105.5% with an RSD no more than 2.77%. These quantification results of seven compounds determined in the samples were further confirmed by HPLC-QTOF-MS/MS. This study provides a useful and simple method for analyzing the major bioactive compounds and improves the quality assessment research of KXP.
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Project description:(1) Background: Metabolism data of asarone isomers, in particular phase II, in vitro and in humans is limited so far. For the first time, phase II metabolites of asarone isomers were characterized and human kinetic as well as excretion data after oral intake of asarone-containing tea infusion was determined. (2) Methods: A high pressure liquid chromatography coupled with quadrupole time-of-flight mass spectrometry (HPLC-qTOF-MS) approach was used to identify phase II metabolites using liver microsomes of different species and in human urine samples. For quantitation of the respective glucuronides, a beta-glucuronidase treatment was performed prior to analysis via high pressure liquid chromatography coupled with tandem mass spectrometry (HPLC-MS/MS). (3) Results: Ingested beta-asarone and erythro and threo-asarone diols were excreted as diols and respective diol glucuronide conjugates within 24 h. An excretion rate about 42% was estimated. O-Demethylation of beta-asarone was also indicated as a human metabolic pathway because a corresponding glucuronic acid conjugate was suggested. (4) Conclusions: Already reported O-demethylation and epoxide-derived diols formation in phase I metabolism of beta-asarone in vitro was verified in humans and glucuronidation was characterized as main conjugation reaction. The excretion rate of 42% as erythro and threo-asarone diols and respective asarone diol glucuronides suggests that epoxide formation is a key step in beta-asarone metabolism, but further, as yet unknown metabolites should also be taken into consideration.
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Project description:Background:Danmu preparations (Danmu Capsule and Danmu Syrup), which are made from Nauclea officinalis stem extracts, have good clinical efficacy in acute tonsillitis, acute pharyngitis and upper respiratory tract infection. However, there is currently no reliable and systematic method to control the quality of these two Danmu preparations. Methods:Using high-performance liquid chromatography (HPLC) coupled with diode array detection (DAD), the fingerprints of the Danmu preparations were established at 250 nm to comprehensively investigate the stability of preparation process. The chemical constituents in the Danmu preparations were separated and identified by HPLC coupled with quadrupole-time-of-flight high-definition mass spectrometry (HPLC-Q-TOF-MS). And seven major components were simultaneously determined at dual wavelengths (250 nm, 326 nm). Results:The results of HPLC fingerprint similarity evaluation showed that the similarity values of 25 batches of Danmu preparations were more than 0.993. Twenty-three compounds, including 10 alkaloids, 6 phenolic acids, 2 iridoids, and 5 unknown compounds, were identified or tentatively characterized according to the retention times and MS/MS fragment patterns of compounds. The developed assay method of seven components was validated with acceptable linearity, precision, repeatability, stability and recovery. The contents of strictosamide belonging to alkaloids as the most abundant constituent in Danmu Capsule and Danmu Syrup were 43,681.20-99,652.49 ?g/g and 1567.83-2427.25 ?g/mL respectively. The contents of protocatechuic acid which were the highest in measured phenolic acids were 2633.01-7739.78 ?g/g in Danmu Capsule and 192.05-448.71 ?g/mL in Danmu Syrup, respectively. As an iridoid, the contents of sweroside in Danmu Capsule and Danmu Syrup were 1573.82-2789.81 ?g/g and 70.32-182.81 ?g/mL, respectively. Conclusion:The established qualitative analysis method of fingerprint can be used to attain standardization, uniformity and stability of the preparation process. Meanwhile, the quantitative analysis in this study can be used as an accurate assay method for preparations.
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Project description:BackgroundSiwu decoction categorized formulae (SWDCF) are widely used for treating gynecological diseases. This study aims to elucidate the differences of bioactive constituents in SWDCF by ultra-high performance liquid chromatography coupled with time-of-flight mass spectrometry (UPLC - QTOF - MS /MS) and HPLC-DAD.MethodsAn efficient method based on UPLC - QTOF - MS /MS was developed for identifying the chemical profiles of SWDCF. HPLC-DAD method was used for quantifying seven chemical markers in SWDCF.ResultsEighty four components were identified or characterized, including ten organic acids, thirty glycosides (monoterpene or iridoid or phenylpropanoids glycosides), fourteen lactones, eighteen flavonoids, and eleven alkaloids in the complex system. The datasets of tR-m/z pairs, ion intensities and sample codes were processed with supervised orthogonal partial least squared discriminant analysis to compare these decoction samples. After a clear classification was established, OPLS-DA was performed and 16 common components with relative quantity in SWDCF samples were determined. Gallic acid, protocatechuic acid, vanillic acid, caffeic acid, paeoniflorin, ferulic acid, and senkyunolide I were selected as the chemical markers to identify SWDCF by HPLC-DAD.ConclusionThe chemical profiles with 84 components in SWDCF, including monoterpene glycosides, acetophenones, galloyl glucoses, even some isomers in the complex system were characterized by UPLC-QTOF-MS/MS.
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Project description:Commercial preparations of Ginkgo biloba are very complex mixtures prepared from raw leaf extracts by a series of extraction and prepurification steps. The pharmacological activity is attributed to a number of flavonoid glycosides and unique terpene trilactones (TTLs), with largely uncharacterized pharmacological profiles on targets involved in neurological disorders. It is therefore important to complement existing targeted analytical methods for analysis of Ginkgo biloba preparations with alternative technology platforms for their comprehensive and global characterization. In this work, (1)H NMR-based metabolomics and hyphenation of high-performance liquid chromatography, photo-diode array detection, mass spectrometry, solid-phase extraction, and nuclear magnetic resonance spectroscopy (HPLC-PDA-MS-SPE-NMR) were used for investigation of 16 commercially available preparations of Ginkgo biloba. The standardized extracts originated from Denmark, Italy, Sweden, and United Kingdom, and the results show that (1)H NMR spectra allow simultaneous assessment of the content as well as identity of flavonoid glycosides and TTLs based on a very simple sample-preparation procedure consisting of extraction, evaporation and reconstitution in acetone-d(6). Unexpected or unwanted extract constituents were also easily identified in the (1)H NMR spectra, which contrasts traditional methods that depend on UV absorption or MS ionizability and usually require availability of reference standards. Automated integration of (1)H NMR spectral segments (buckets or bins of 0.02 ppm width) provides relative distribution plots of TTLs based on their H-12 resonances. The present study shows that (1)H NMR-based metabolomics is an attractive method for non-selective and comprehensive analysis of Ginkgo extracts. ELECTRONIC SUPPLEMENTARY MATERIAL: The online version of this article (doi:10.1007/s11306-009-0195-x) contains supplementary material, which is available to authorized users.
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Project description:Rhodoterpenoids A?C (1?3), three new rearranged triterpenoids, together with one new biogenetically related compound, rhodoterpenoid D (4), were isolated and efficiently elucidated from Rhododendron latoucheae by high-performance liquid chromatography-mass spectrometry-solid-phase extraction-nuclear magnetic resonance (HPLC?MS?SPE?NMR). Compounds 1 and 2 possess an unprecedented skeleton with a 5/7/6/6/6-fused pentacyclic ring system, while compound 3 contains a unique 6/7/6/6/6-fused pentacyclic carbon backbone. Their structures were determined by extensive spectroscopic methods and electronic circular dichroism (ECD) analyses. Plausible biogenetic pathways for 1?4 were proposed. Compounds 1 and 4 showed potential activity against herpes simplex virus 1 (HSV-1) with IC50 values of 8.62 and 6.87??M, respectively.
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Project description:Glucosinolates are well known as natural antimicrobials and anticarcinogenic agents. However, these compounds can lose their properties and transform into antinutrients, depending on processing conditions. In addition, the bitterness of some glucosinolate in rapeseed meal can affect the likability of the final product. Therefore, it is important to identify and determine each glucosinolate and its derived form, not just the total glucosinolate content, in order to evaluate the potential of the final rapeseed protein product. This study provides a comprehensive report of the types and quantities of glucosinolates and their derived forms (isothiocyanates) associated with different rapeseed processing conditions. Glucosinolates and isothiocyanates were determined by HPLC-DAD-qTOF. In our study, the enzymatic degradation of glucosinolates by myrosinase was the main factor affecting either glucosinolate or isothiocyanate content. Other factors such as pH seemed to influence the concentration and the presence of glucosinolates. In addition, process parameters, such as extraction time and separation technology, seemed to affect the amount and type of isothiocyanates in the final protein extracts. Overall, both determined intact glucosinolates and their derived forms of isothiocyanates can give different types of biological effects. More studies should be performed to evaluate the impact of glucosinolates and isothiocyanates on human health.
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Project description:Ginsenosides are the characteristic and principal components which manifest a variety of the biological and pharmacological activities of the roots and rhizomes of Panax ginseng (GRR). This study was carried out to qualitatively and quantitatively determine the ginsenosides in the cultivated and forest GRR.A rapid and sensitive ultra-high-performance liquid chromatography coupled with diode-array detector and quadrupole/time of flight tandem mass spectrometry (UPLC-DAD-QTOF-MS/MS) was applied to the qualitative analysis of ginsenosides and a 4000 QTRAP triple quadrupole tandem mass spectrometer (HPLC-ESI-MS) was applied to quantitative analysis of 19 ginsenosides.In the qualitative analysis, all ingredients were separated in 10 min. A total of 131 ginsenosides were detected in cultivated and forest GRR. The method for the quantitative determination was validated for linearity, precision, and limits of detection and quantification. 19 representative ginsenosides were quantitated. The total content of all 19 ginsenosides in the forest GRR were much higher than those in the cultivated GRR, and were increased with the growing ages.This newly developed analysis method could be applied to the quality assessment of GRR as well as the distinction between cultivated and forest GRR.
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Project description:Fringed sagewort (Artemisia frigida Willd., Compositae family) is a well-known medicinal plant in Asian medical systems. Fifty-nine hydroxycinnamates and flavonoids have been found in A. frigida herbs of Siberian origin by high-performance liquid chromatography with diode array and electrospray triple quadrupole mass detection (HPLC-DAD-ESI-QQQ-MS). Their structures were determined after mass fragmentation analysis as caffeoylquinic acids, flavone O-/C-glycosides, flavones, and flavonol aglycones. Most of the discovered components were described in A. frigida for the first time. It was shown that flavonoids with different types of substitution have chemotaxonomic significance for species of Artemisia subsection Frigidae (section Absinthium). After HPLC-DAD quantification of 16 major phenolics in 21 Siberian populations of A. frigida and subsequent principal component analysis, we found substantial variation in the selected compounds, suggesting the existence of two geographical groups of A. frigida. The antioxidant activity of A. frigida herbal tea was determined using 2,2-diphenyl-1-picrylhydrazyl free radical (DPPH•) and hydrophilic/lipophilic oxygen radical absorbance capacity (ORAC) assays and DPPH•-HPLC profiling, revealing it to be high. The effect of digestive media on the phenolic profile and antioxidant capacity of A. frigida herbal tea was assessed under simulated gastrointestinal digestion. We found a minor reduction in caffeoylquinic acid content and ORAC values, but remaining levels were satisfactory for antioxidant protection. These results suggest that A. frigida and its food derivate herbal tea could be recommended as new plant antioxidants rich in phenolics.
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Project description:Mediterranean plant Helichrysum italicum represents a rich source of versatile bioactive compounds with potential benefits for human health. Despite extensive research on the plant's active constituents, little attention has yet been paid to characterizing the relationship between its intra-specific genetic diversity and metabolite profile. The study aimed to determine metabolic profile of H. italicum ssp. italicum (HII) and ssp. tyrrhenicum (HIT) cultivated on the experimental plantation in Slovenia and to compare the chemical composition of extracts regarding the solvent extraction process. Extracts were prepared upon conventional extract preparation procedures: maceration with 50 % methanol or ethanol and cold or hot water infusion and analyzed using High Performance Liquid Chromatography-Diode Array Detection-Electrospray Ionization-Quadrupole Time-of-Flight-Mass Spectrometry (HPLC-DAD-ESI-QTOF-MS). One hundred compounds were identified in the samples, among them several isomers and derivatives were reported for the first time, while caffeoylquinic acids and pyrones were the most abundant. Semi-quantitative comparison revealed that the extraction procedure had a greater impact on the chemical profile than genetic variability. All HIT extracts showed a higher total phenolic content compared to HII, while the antioxidant potential evaluated by 1,1-diphenyl-2-picrylhydrazil test was not proportionally higher. In addition, hot water extracts proved to be comparably active as alcoholic ones, confirming high commercial potential of Helichrysum italicum as herbal functional beverages.
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