RESUMEN

Curcumae Radix (CR) is a widely used traditional Chinese medicine with significant pharmaceutical importance, including enhancing blood circulation and addressing blood stasis. This study aims to establish an integrated and rapid quality assessment method for CR from various botanical origins, based on chemical components, antiplatelet aggregation effects, and Fourier transform near-infrared (FT-NIR) spectroscopy combined with multivariate algorithms. Firstly, ultra-performance liquid chromatography-photodiode array (UPLC-PDA) combined with chemometric analyses was used to examine variations in the chemical profiles of CR. Secondly, the activation effect on blood circulation of CR was assessed using an in vitro antiplatelet aggregation assay. The studies revealed significant variations in chemical profiles and antiplatelet aggregation effects among CR samples from different botanical origins, with constituents such as germacrone, ß-elemene, bisdemethoxycurcumin, demethoxycurcumin, and curcumin showing a positive correlation with antiplatelet aggregation biopotency. Thirdly, FT-NIR spectroscopy was integrated with various machine learning algorithms, including Artificial Neural Network (ANN), K-Nearest Neighbors (KNN), Logistic Regression (LR), Support Vector Machine (SVM), and Subspace K-Nearest Neighbors (Subspace KNN), to classify CR samples from four distinct sources. The result showed that FT-NIR combined with KNN and SVM classification algorithms after SNV and MSC preprocessing successfully distinguished CR samples from four plant sources with an accuracy of 100%. Finally, Quantitative models for active constituents and antiplatelet aggregation bioactivity were developed by optimizing the partial least squares (PLS) model with interval combination optimization (ICO) and competitive adaptive reweighted sampling (CARS) techniques. The CARS-PLS model achieved the best predictive performance across all five components. The coefficient of determination (R2p) and root mean square error (RMSEP) in the independent test sets were 0.9708 and 0.2098, 0.8744 and 0.2065, 0.9511 and 0.0034, 0.9803 and 0.0066, 0.9567 and 0.0172 for germacrone, ß-elemene, bisdemethoxycurcumin, demethoxycurcumin and curcumin, respectively. The ICO-PLS model demonstrated superior predictive capabilities for antiplatelet aggregation biotency, achieving an R2p of 0.9010, and an RMSEP of 0.5370. This study provides a valuable reference for the quality evaluation of CR in a more rapid and comprehensive manner.

Asunto(s)

Curcuma , Inhibidores de Agregación Plaquetaria , Agregación Plaquetaria , Espectroscopía Infrarroja Corta , Curcuma/química , Espectroscopía Infrarroja Corta/métodos , Agregación Plaquetaria/efectos de los fármacos , Espectroscopía Infrarroja por Transformada de Fourier/métodos , Inhibidores de Agregación Plaquetaria/análisis , Inhibidores de Agregación Plaquetaria/química , Animales , Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Algoritmos , Extractos Vegetales/química

RESUMEN

Given the limited specificity and accuracy observed in the current official colorimetric quantification of polysaccharide in Lycium barbarum, our study aims to establish a novel, specific, accurate, and economic pre-column derivatization ultra-high-performance liquid chromatography (UHPLC) method for determining the monosaccharide and polysaccharide content in L. barbarum. The optimization of extraction, hydrolysis, and derivatization (using 1-phenyl-3-methyl-5-pyrazolone) processes for polysaccharide from L. barbarum was conducted initially, followed by separation of nine monosaccharides within 20 min using UHPLC with a C18 column. Subsequently, a novel method known as quantitative analysis of multiple components by single marker was developed, utilizing either additive 2-deoxy-D-ribose or any monosaccharide present in the sample as a single reference standard to simultaneously detect the contents of polysaccharide and nine monosaccharides in L. barbarum. To validate the accuracy of the established method, the quantitative results of our approach were compared to both external and internal standard method methods. The minimal relative errors in the quantitative determination of monosaccharides among the three methods confirmed the dependability of the method. By analyzing 20 batches of L. barbarum samples, D-galacturonic acid exhibited the highest content and the polysaccharide levels ranged from 3.02 to 13.04 mg/g. All data implied the specificity and accuracy of the method.

Asunto(s)

Lycium , Monosacáridos , Polisacáridos , Cromatografía Líquida de Alta Presión/métodos , Lycium/química , Monosacáridos/análisis , Monosacáridos/química , Polisacáridos/análisis , Polisacáridos/química , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis

RESUMEN

BACKGROUND: The Atractylodes chinensis (DC.) Koidz (A. chinensis) Chinese herb possesses numerous therapeutic properties and is extensively utilized in the pharmaceutical industry. Its quality is closely associated with the harvest periods. However, the optimal quality and harvest periods of A. chinensis remain elusive. METHODS: The bioactive compounds of perennial A. chinensis were detected by ultra-high-performance liquid chromatography coupled with quadrupole Orbitrap mass spectrometry (UHPLC-Q-Orbitrap/MS) metabolomics, and differentially abundant compounds were selected by multivariate statistical analysis. Then, variations in the content of differential compounds in samples harvested at different periods were analyzed, while correlation analysis was carried out on the differential compounds to determine the suitable harvest period for distinct components. RESULTS: A total of 61 bioactive compounds were detected in all samples, grouped into 9 known classes. The results revealed that the chemical compositions of A. chinensis at different harvest periods were significantly different. The volatile oil content in the four-year-old and five-year-old samples was relatively high, at 31.92 mg/g and 32.42 mg/g, respectively. There were also significant differences in the content of the six active ingredients, for example, the five-year-old sample had the highest content of atractylodin (4.38 mg/g). Indeed, the harvest period was correlated with the abundance of most bioactive compounds. Specifically, quinquennial samples were significantly negatively correlated with the abundance of organic acids and aliphatics while moderately positively correlated with the abundance of other classes of bioactive compounds. CONCLUSIONS: According to the results, the ideal harvest time for atractylenolide Ⅲ was 3 years. Regarding organic acids, the optimal harvest time was around 2-3 years. Taken together, these results offer valuable insights to producers for optimizing the harvest period for A. chinensis.

Asunto(s)

Atractylodes , Atractylodes/química , Cromatografía Líquida de Alta Presión/métodos , Análisis Multivariante , Sesquiterpenos/análisis , Lactonas/análisis , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Aceites Volátiles/análisis , Aceites Volátiles/química , Espectrometría de Masas/métodos , Metabolómica/métodos

RESUMEN

Angelicae sinensis radix (ASR) and Angelicae pubescentis radix (APR), as traditional herbal medicines, are often confused and doped in the material market. However, the traditional identification method is to characterize the whole herb with a single or a few components, which do not have representation and cannot realize the effective utilization of unknown components. Consequently, the result is not convincing. In addition, the whole process is time-consuming and labor-intensive. To avoid the confusion and adulteration of ASR and APR as well as to strengthen quality control and improve identification efficiency, in this study, a UHPLC-QTOF-MSE method was used to analyze ASR and APR. Based on digital representation, the shared data with high ionic strength were extracted from different batches of the same herbal medicine as their "digital identity". Further, the above "digital identity" was used as the benchmark for matching and identifying unknown samples to feedback on matching credibility (MC). The results showed that based on the "digital identities" of ASR and APR, the digital identification of two herbal samples can be realized efficiently and accurately at the individual level. And the matching credibility (MC) was higher than 94.00%, even if only 1% of APR or ASR in the mixed samples can still be identified efficiently and accurately. The study is of great practical significance for improving the efficiency of the identification of ASR and APR, cracking down on adulterated and counterfeit drugs, and strengthening the quality control of ASR and APR. In addition, it has important reference significance for developing nontargeted digital identification of herbal medicines at the individual level based on UHPLC-QTOF-MSE and "digital identity", which is beneficial to the construction of digital Chinese medicine and digital quality control.

Asunto(s)

Angelica sinensis , Medicamentos Herbarios Chinos , Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Angelica sinensis/química , Espectrometría de Masas/métodos , Control de Calidad , Raíces de Plantas/química , Angelica/química

RESUMEN

BACKGROUND: The proposal of Q-markers for traditional Chinese medicine (TCM) represents a novel avenue of research pertaining to the quality control of TCM prescriptions. However, prior exploratory studies on Q-markers with multiple properties consistently neglected the consideration of weights, hampering our ability to accurately gauge the significance of each property and potentially leading to a flawed comprehension of Q-markers. PURPOSE: In this study, a quantitative ternary network strategy was firstly proposed to visually discover the Q-markers from TCM prescriptions, and it has been successfully applied into the quality control study of Bu-Zhong-Yi-Qi-Tang (BZYQT), a classical TCM prescription. METHODS: Firstly, the contents of 34 components in BZYQT, along with the kinetic features of 17 candidate Q-markers in biosamples (plasma and small intestinal contents), were characterized by UPLC-QqQ-MS/MS, and their immunomodulatory activities in macrophages and splenic lymphocytes were also assessed. Next, the obtained data were integrated into three properties: testability, bioavailability, effectiveness, and their weights were calculated using the entropy weight method to further establish a ternary network for quantitatively screening Q-markers. Subsequently, the identified Q-markers of BZYQT were utilized for the holistic quality evaluation of 36 batches of the commercial BZYQT preparation, Bu-Zhong-Yi-Qi-Pill (BZYQP) produced by three manufacturers, through similarity evaluation of the Q-marker-based fingerprint. RESULTS: Nine compounds (hesperidin, astragaloside IV, ononin, 18ß-glycyrrhizic acid, narirutin, calycosin, cimigenoside, astragaloside II, and liquiritin) showing three core properties, including testability, bioavailability, and effectiveness, were screened out as Q-markers of BZYQT based on their rankings in terms of regression area of the ternary network. Employing Q-markers as common peaks, the similarity values of 36 batches BZYQP ranged 0.914-0.998 under HPLC-UVD mode, and 0.631-1.000 under HPLC-ELSD mode, which were less than the similarity values evaluated by the conventional common peaks (HPLC-UVD mode: 0.946-0.990; HPLC-ELSD mode: 0.957-0.997). This observation suggests that the identified Q-markers are more representative as common peaks in chromatographic fingerprints for the holistic quality evaluation of TCM-related products from different manufacturers. CONCLUSION: The quantitative discovery of Q-markers from BZYQT laid an important foundation for holistic quality assessment of its related commercially available products, and our work offering a new strategy for ensuring the consistency and efficacy of TCM prescriptions.

Asunto(s)

Medicamentos Herbarios Chinos , Medicina Tradicional China , Medicamentos Herbarios Chinos/farmacología , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Animales , Cromatografía Líquida de Alta Presión/métodos , Control de Calidad , Espectrometría de Masas en Tándem/métodos , Masculino , Ratones

RESUMEN

Under the background of digitalization of traditional Chinese medicine (TCM), to realize the quick identification and adulteration analysis of Pulsatilla Radix (PR), adhering to digital conviction, this study conducted UHPLC-QTOF-MSE analysis on PR and its adulterant-Pulsatilla Cernua (PC) from different batches and based on digital conversion, the shared ions were extracted from different batches of PR and PC as their "ions representation", respectively. Further, the data set of unique ions of PR relative to PC and PC relative to PR were screened out as the "digital identities" of PR and PC respectively. Further, above the "digital identities" of PR and PC were used as the benchmarks for matching and identifying to feedback give a matching credibility (MC). The results showed that based on the "digital identities" of PR and PC, the digital identification of two herbal samples can be realized efficiently and accurately at the individual level with the MC≥70.00 %, even if 5 % of PC in the mixed samples can still be identified efficiently and accurately. The study is of great practical significance for improving the identification efficiency of PR and PC, cracking down on adulterated and counterfeit drugs, and strengthening the quality control of PR. In addition, it has important reference significance for developing non-targeted digital identification of herbal medicines at the individual level based on UHPLC-QTOF-MSE and the "digital identity", which was beneficial to the construction of digital Chinese medicine and digital quality control.

Asunto(s)

Contaminación de Medicamentos , Medicamentos Herbarios Chinos , Pulsatilla , Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Pulsatilla/química , Espectrometría de Masas/métodos , Reproducibilidad de los Resultados

RESUMEN

In this work, electromembrane extraction (EME) was used for the first time to separate aconitine (AC), mesaconitine (Mes-AC) and hypaconitine (Hyp-AC) from biological samples and Chinese herbal medicines. Efficient EME of polar and high molecular weight aconitine alkaloids from different sample matrices was achieved with the solvent of 1-ethyl-2-nitrobenzene (ENB). Under the optimal EME conditions, EME provided recoveries for all targets in the range of 72%-74 %, 85%-103 % and 92%-94 % for whole blood, urine and aqueous samples. The proposed EME systems combined with LC-MS/MS and HPLC-UV were evaluated using different sample matrices, and the methods displayed satisfactory analytical characteristic including negligible matrix effect. The LOD and LOQ of AC, Mes-AC, and Hyp-AC by EME-LC-MS/MS were in the range of 0.002-0.068 ng/mL and 0.005-0.228 ng/mL respectively. The LOD and LOQ of AC, Mes-AC, and Hyp-AC by EME-HPLC-UV were in the range of 0.06-0.26 µg/mL and 0.20-0.86 µg/mL, respectively. The coefficient of determination, R2-value was ≥0.9926 for all cases, and the accuracy in the linear ranges was in the range of 91%-111 %. Finally, the method was successfully applied for the qualitative and quantitative analysis of AC and Mes-AC in the whole blood and herbal medicine dreg samples from an actual forensic case, and poisoning by aconitum alkaloids was identified as the cause of death. Therefore, we believe that EME could be a powerful tool to identify poisoning, and EME has great potential for efficient separation of polar and high molecular weight substances. These are of great importance in the fields of but not limited to forensic science, Traditional Chinese Medicine and clinics.

Asunto(s)

Aconitum , Humanos , Aconitum/química , Aconitum/envenenamiento , Alcaloides/análisis , Alcaloides/orina , Alcaloides/sangre , Membranas Artificiales , Espectrometría de Masas en Tándem/métodos , Técnicas Electroquímicas , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Cromatografía Líquida de Alta Presión , Aconitina/análogos & derivados , Aconitina/análisis , Aconitina/sangre , Fraccionamiento Químico/métodos , Límite de Detección

Asunto(s)

Antioxidantes , Medicamentos Herbarios Chinos , Antioxidantes/química , Antioxidantes/análisis , Antioxidantes/farmacología , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/farmacología , Medicamentos Herbarios Chinos/análisis , Astragalus propinquus/química , Control de Calidad , Planta del Astrágalo/química , Cromatografía Líquida de Alta Presión , Raíces de Plantas/química , Raíces de Plantas/crecimiento & desarrollo

RESUMEN

Magnolia bark is a traditional Chinese medicine used for hypoglycaemia. With the widespread use of Magnolia bark, its resources are facing a serious shortage. To address this issue, a strategy based on high-coverage mass spectrometry (HCMS) and multidimensional chemical-biological analysis (MCBA) was proposed for the comprehensive exploration of Magnolia officinalis which is the main source of Magnolia bark. The strategy is divided into three main steps. In the first step, the stem bark, stem xylem, root bark, root xylem, leaf and rootlet of Magnolia officinalis were comprehensively analyzed using high-coverage mass spectrometry. In the second step, multivariate statistical analysis was used to explore the heterogeneity of the six parts and detect differential chemical components. In the third step, a combination of experimental screening and molecular docking was used to explore α-glucosidase inhibitors from Magnolia officinalis. Multidimensional chemical-biological analysis (MCBA) of Magnolia officinalis was achieved by combining the last two steps. Finally, a total of 103 compounds were identified from the whole plant of Magnolia officinalis. Differential components of stem bark, stem xylem, leaf, root bark, root xylem and rootlet were systematically revealed. A pair of positional isomers, namely magnolol and honokiol, were found to be α-glucosidase inhibitors. The activity of their combination is superior to that of each single compound, indicating that magnolol and honokiol are in a synergistic relationship. This strategy contributes to comprehensive exploitation of functional plants and effective alleviation of resource shortage. This study also provides a research paradigm for other similar traditional Chinese medicinal plants.

Asunto(s)

Magnolia , Espectrometría de Masas , Magnolia/química , Espectrometría de Masas/métodos , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Simulación del Acoplamiento Molecular , Plantas Medicinales/química , Inhibidores de Glicósido Hidrolasas/análisis , Inhibidores de Glicósido Hidrolasas/química

RESUMEN

Cis-trans isomers of N-isobutyl-2E,4E,8Z,10E-dodecatetraenamide (DDA-E) and N-isobutyl-2E,4E,8Z,10Z-dodecatetraenamide (DDA-Z) are representative alkamides with numbness of tongue, anti-inflammatory and analgesic activities of Asari Radix et Rhizoma. However, their respective metabolic pathways and pharmacokinetic behaviors are still unknown. This study aim to investigate the metabolism of the two alkamides in vitro and in vivo using ultra-high-performance liquid chromatography-quadruple-time-of-flight mass spectrometry. Furthermore, a rapid, sensitive, and selective ultra-high-performance liquid chromatography-tandem mass spectrometry method was developed to quantify DDA-E/Z in rat plasma. Results indicated that DDA-E and DDA-Z showed significant differences in metabolism and pharmacokinetics. Across all samples, 24 metabolites of DDA-E and 21 metabolites of DDA-Z were detected. A variety of pathways were involved in the production of these metabolites, mainly hydroxylation and oxidation. The linear range of DDA-E/Z was 1-2500 ng/mL (R2 = 0.9984), and the lowest quantification limit was 1 ng/mL. Precision, accuracy, extraction recovery, matrix effect, and stability of DDA-E/Z were within acceptable limits. Pharmacokinetic research was conducted using male Sprague-Dawley rats receiving intravenous (1 mg/kg) or intragastric (40 mg/kg) administration of DDA-E or DDA-Z solution. There was a calculated absolute bioavailability of 15.67 % for DDA-E and 4.83 % for DDA-Z when consumed orally. The apparent volume of distribution of intravenous and intragastric administrations were 4.44 ± 0.41 L/kg and 5.18 ± 0.67 L/kg for DDA-E, and 1.56 ± 1.66 L/kg and 2.35 ± 0.42 L/kg for DDA-Z. The maximal plasma concentrations of DDA-E and DDA-Z were 599.84 ± 149.92 nM and 422.09 ± 69.17 nM, and the time to maximum peak were 4.33 ± 3.51 h and 0.70 ± 1.12 h, respectively. In conclusion, in subsequent pharmacodynamics and safety evaluation studies, great attention should be paid to the metabolic characteristics and pharmacokinetic differences between DDA-E and DDA-Z.

Asunto(s)

Medicamentos Herbarios Chinos , Ratas Sprague-Dawley , Espectrometría de Masas en Tándem , Animales , Espectrometría de Masas en Tándem/métodos , Cromatografía Líquida de Alta Presión/métodos , Masculino , Ratas , Medicamentos Herbarios Chinos/farmacocinética , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/administración & dosificación , Medicamentos Herbarios Chinos/análisis , Isomerismo , Rizoma/química , Microsomas Hepáticos/metabolismo , Administración Oral

RESUMEN

In traditional Chinese medicinal practices, Gegen (GG) and Tianma (TM) are widely utilized for headache relief, but their material basis has not been comprehensively characterized. This research utilized ultra performance liquid chromatography-quadrupole-time of flight-mass spectrometry (UPLC-Q-TOF-MS) for precise determination of Gegen-Tianma's (GGTM) material composition, and employed desorption electrospray ionization-mass spectrometry imaging (DESI-MSI) to pinpoint the brain-absorbed components and various metabolites post oral administration to rats. A total of 80 chemical constituents were identified from GGTM, 11 prototypes and 18 metabolites were identified from plasma. The brain tissue was identified in total 4 prototypes and 5 metabolites, these constituents were basically located in the prefrontal cortex and thalamus. The absorption patterns of components in the rat brain aligned with the varied distribution of metabolites within the brain. This study provides a solid theoretical basis for in-depth exploration of potential drug targets and elucidation of the specific mechanism of action of GGTM in the treatment of migraine.

Asunto(s)

Encéfalo , Medicamentos Herbarios Chinos , Ratas Sprague-Dawley , Espectrometría de Masa por Ionización de Electrospray , Animales , Medicamentos Herbarios Chinos/farmacocinética , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Ratas , Cromatografía Líquida de Alta Presión/métodos , Masculino , Encéfalo/metabolismo , Espectrometría de Masa por Ionización de Electrospray/métodos , Administración Oral , Corteza Prefrontal/metabolismo , Distribución Tisular

RESUMEN

Astragalus membranaceus (A. membranaceus) leaves can be used both as a medicine and food material. Their main chemical components are flavonoids and triterpenoid saponins. The pharmacokinetics of A. membranaceus leaves are rarely reported in the literature. This study aimed to investigate the pharmacokinetics of five major bioactive components of A. membranaceus leaves [rhamnocitrin 3-glucoside (RCG), tiliroside (TIL), rhamnocitrin 3-neohesperidoside (RNH), huangqiyenin R (HuR), and huangqiyenin I (HuI)]. Simultaneously using ultra-high-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS/MS) method. The extract of A. membranaceus leaves was administered orally to rats, and the rat plasma was subjected to a fast, sensitive, and specific UHPLC-MS/MS method. Butylparaben served as the internal standard. The plasma samples were pretreated using isopropanol/ethyl acetate (1:1, v/v) liquid-liquid extraction. Chromatographic separations were performed at a flow rate of 0.3 mL/min on a Waters ACQUITY HSS T3 Column (2.1 mm × 100 mm, 1.8 µm) using mobile phases of 0.1 % formic acid/water and 0.1 % formic acid/acetonitrile. Mass spectrometry detection was performed using an electrospray ionization ion source in the negative-ion mode and the multiple reaction monitoring mode. All analytes had an intraday and interday relative standard deviation of less than 14.10 %. The range of accuracy was -11.94-6.920 % and -15.22-5.800 %. The lower limits of quantification for RCG, TIL, RNH, HuR, HuI was 10.24, 10.27, 10.12, 5.137, and 5.841 ng/mL, respectively. The criteria were met by stability, matrix effects, and extraction recovery. The pharmacokinetic parameters of A. membranaceus leaf extract were ultimately obtained using this analytical method. The study provides a theoretical basis for future pharmacological research, clinical application, and development of healthy food from A. membranaceus leaves.

Asunto(s)

Astragalus propinquus , Flavonoides , Hojas de la Planta , Ratas Sprague-Dawley , Saponinas , Espectrometría de Masas en Tándem , Triterpenos , Espectrometría de Masas en Tándem/métodos , Cromatografía Líquida de Alta Presión/métodos , Hojas de la Planta/química , Animales , Flavonoides/farmacocinética , Flavonoides/sangre , Flavonoides/análisis , Saponinas/farmacocinética , Saponinas/sangre , Saponinas/análisis , Ratas , Triterpenos/farmacocinética , Triterpenos/sangre , Triterpenos/análisis , Masculino , Extractos Vegetales/farmacocinética , Extractos Vegetales/química , Medicamentos Herbarios Chinos/farmacocinética , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Administración Oral , Reproducibilidad de los Resultados

RESUMEN

Shaoyao Gancao Decoction (SGD), a traditional Chinese medicine, has been proven to have a good liver protection effect, but the mechanism and pharmacodynamic substances of SGD in the treatment of acute liver injury are still unclear. In this study, an ultra-high-performance liquid chromatography-quadrupole-time-of-flight mass spectrometry (UHPLC-Q-TOF-MS) method was established to characterize 107 chemical components of SGD and 12 compounds absorbed in rat plasma samples after oral administration of SGD. Network pharmacology was applied to construct a component-target-pathway network to screen the possible effective components of SGD in acute liver injury. Using lipidomics based on UHPLC-Q-TOF-MS coupled with a variety of statistical analyses, 20 lipid biomarkers were screened and identified, suggesting that the improvement of acute liver injury by SGD was involved in cholesterol metabolism, glycerol-phospholipid metabolism, sphingolipid signaling pathways and fatty acid biosynthesis. In addition, the UHPLC-tandem MS method was established for pharmacokinetics analysis, and 10 potential active components were determined simultaneously within 12 min through the optimization of 0.1% formic acid water and acetonitrile as a mobile phase system. A Pharmacokinetics study showed that paeoniflorin, albiflorin, oxypaeoniflorin, liquiritigenin, isoliquiritigenin, liquiritin, ononin, formononetin, glycyrrhizic acid, and glycyrrhetinic acid as the potential active compounds of SGD curing acute liver injury.

Asunto(s)

Medicamentos Herbarios Chinos , Lipidómica , Ratas Sprague-Dawley , Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/farmacocinética , Medicamentos Herbarios Chinos/análisis , Animales , Ratas , Masculino , Lipidómica/métodos , Espectrometría de Masas , Administración Oral , Glucósidos/farmacocinética , Glucósidos/sangre , Medicina Tradicional China , Cromatografía Líquida con Espectrometría de Masas

RESUMEN

Background:Periplocae Cortex (PC), Acanthopanacis Cortex (AC), and Lycii Cortex (LC), as traditional Chinese medicines, are all dried root bark, presented in a roll, light and brittle, easy to break, have a fragrant scent, etc. Due to their similar appearances, it is tough to distinguish them, and they are often confused and adulterated in markets and clinical applications. To realize the identification and quality control of three herbs, in this paper, Ultra Performance Liquid Chromatography-Quadrupole Time of Flight Mass Spectrometry Expression (UHPLC-QTOF-MSE) combined with chemometric analysis was used to explore the different chemical compositions. Methods: LC, AC, and PC were analyzed by UHPLC-QTOF-MSE, and the quantized MS data combined with Principal Component Analysis (PCA) and Partial Least Squares Discriminant Analysis (PLS-DA) were used to explore the different chemical compositions with Variable Importance Projection (VIP) > 1.0. Further, the different chemical compositions were identified according to the chemical standard substances, related literature, and databases. Results: AC, PC, and LC can be obviously distinguished in PCA and PLS-DA analysis with the VIP of 2661 ions > 1.0. We preliminarily identified 17 differential chemical constituents in AC, PC, and LC with significant differences (p < 0.01) and VIP > 1.0; for example, Lycium B and Periploside H2 are LC and PC's proprietary ingredients, respectively, and 2-Hydroxy-4-methoxybenzaldehyde, Periplocoside C, and 3,5-Di-O-caffeoylquinic acid are the shared components of the three herbs. Conclusions: UHPLC-QTOF-MSE combined with chemometric analysis is conducive to exploring the differential chemical compositions of three herbs. Moreover, the proprietary ingredients, Lycium B (LC) and Periploside H2 (PC), are beneficial in strengthening the quality control of AC, PC, and LC. In addition, limits on the content of shared components can be set to enhance the quality control of LC, PC, and AC.

Asunto(s)

Medicamentos Herbarios Chinos , Espectrometría de Masas , Análisis de Componente Principal , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Cromatografía Líquida de Alta Presión/métodos , Espectrometría de Masas/métodos , Quimiometría , Análisis Discriminante , Análisis de los Mínimos Cuadrados , Corteza de la Planta/química , Medicina Tradicional China

RESUMEN

Traditional Chinese medicine (TCM) and its preparations have become increasingly popular in recent years. Nonetheless, due to the high complexity of the compounds in Traditional Chinese Patent Medicine (TCPM), the quality differences between different dosage forms and products from various manufacturers pose numerous challenges and difficulties in quality evaluation. The Qiangli Tianma Duzhong (QLTMDZ) prescription, comprising twelve TCM, is widely used in China. Despite its prevalence, current research on QLTMDZ is limited and lacks in-depth and systematic analysis of the chemical composition of the prescription. In this study, a comprehensive strategy was proposed for characterizing the chemical profile of QLTMDZ based on UHPLC-Q-TOF-MS. A total of 122 compounds were identified in QLTMDZ under both positive and negative ion modes. Subsequently, multivariate statistical methods such as principal component analysis (PCA) and orthogonal partial least squares-discriminant analysis (OPLS-DA) were conducted in the MS-DIAL software to further elucidate quality differences among 55 batches of QLTMDZ samples from seven manufacturers. Lastly, multiple reaction monitoring (MRM) mode was utilized in conjunction with UHPLC-QQQ-MS, for the precise quantification of the identified 24 compounds within the QLTMDZ preparation and providing supplementary information in quality evaluation. The established analytical method in this study is sensitive and efficient, enabling qualitative and quantitative analysis of the chemical constituents within QLTMDZ. The application of multivariate statistical analyses effectively discriminates samples based on different dosage forms and manufacturers, thereby providing new research directions and scientific support for further studies on the quality control of the prescription.

Asunto(s)

Medicamentos Herbarios Chinos , Medicina Tradicional China , Control de Calidad , Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Medicamentos Herbarios Chinos/normas , Análisis Multivariante , Medicina Tradicional China/normas , Análisis de Componente Principal , Análisis de los Mínimos Cuadrados , Análisis Discriminante , Espectrometría de Masas en Tándem/métodos , Formas de Dosificación , Espectrometría de Masas/métodos , China

RESUMEN

Reduning injection (RDN) is a traditional chinese medicine injection widely used in clinical practice. In this study, qualitative and quantitative analysis of RDN were conducted by UPLC-Orbitrap MS/MS simultaneously. Totally 118 compounds were identified and 34 compounds were quantified in RDN. The method with completed method validation proved the high sensitivity and efficiency of the method and it was applied to quantify compounds in RDN. Multivariate statistical analysis method selected 11 key variables that affect the content consistency of RDN. 20 batches with high biological potency were screened by cox-2 enzyme activity assay. Spectrum-effect relationship analysis and multivariate statistical analysis showed that 7 batches were high-quality selected after comprehensive quality evaluation and 9 compounds were key indicators for screening it. This strategy including fingerprint, qualitative analysis and multiple-component quantification could be well applied to modern quality evaluation of RDN, which could be valuable for the further quality control of more other traditional Chinese medicines.

Asunto(s)

Medicamentos Herbarios Chinos , Control de Calidad , Espectrometría de Masas en Tándem , Espectrometría de Masas en Tándem/métodos , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Cromatografía Líquida de Alta Presión/métodos , Análisis Multivariante , Medicina Tradicional China/métodos , Reproducibilidad de los Resultados

RESUMEN

RATIONALE: Anemarrhenae Rhizoma (AR) has been a frequently utilized traditional Chinese medicine (TCM) for an extended period, with its salt-processed variant being a prevalent application form. Contemporary pharmacological investigations have demonstrated that the salt-processed iteration exhibits a multitude of markedly augmented pharmacological properties. However, whether the pharmacodynamic material basis of this change is related to volatile substances remains unclear. The aim of this study was to develop a strategy to screen volatile pharmacodynamic substances in AR and salt-processed AR (SAR). METHODS: A comprehensive approach was developed to identify volatile pharmacodynamic compounds by integrating plant metabolomics, target network pharmacology, and molecular docking technology. Plant metabolomics using GC-MS analysis was conducted to identify volatile chemical markers distinguishing between AR and SAR. Subsequently, network pharmacology was utilized to investigate the correlation between chemical markers and associated diseases. Following this, molecular docking technology was utilized to explore the correlation between chemical markers and disease targets, resulting in the discovery of potential quality control markers. RESULTS: Fifty volatile compounds were isolated and identified in the salt of AR and SAR. The findings from plant metabolomics analysis demonstrated a distinct differentiation, revealing 13 volatile chemical markers that distinguish between AR and SAR. A target (PPARG) associated with diabetes was identified through target network pharmacology analysis. Thirteen volatile components were subsequently chosen as potential quality markers, taking into account their hypoglycemic activity. CONCLUSIONS: The method developed provides a novel strategy for the identification of pharmacophores in AR and SAR, as well as establishing a foundation for the exploration of the volatile differential components and pharmacodynamics in various processed products of TCMs. Additionally, the findings of this study can serve as a theoretical framework for the development and utilization of volatile components in AR and its processed derivatives.

Asunto(s)

Anemarrhena , Medicamentos Herbarios Chinos , Cromatografía de Gases y Espectrometría de Masas , Metabolómica , Simulación del Acoplamiento Molecular , Rizoma , Compuestos Orgánicos Volátiles , Cromatografía de Gases y Espectrometría de Masas/métodos , Metabolómica/métodos , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/farmacología , Medicamentos Herbarios Chinos/análisis , Compuestos Orgánicos Volátiles/química , Compuestos Orgánicos Volátiles/análisis , Compuestos Orgánicos Volátiles/metabolismo , Rizoma/química , Anemarrhena/química , Farmacología en Red

RESUMEN

Lanbuzheng (Geum japonicum Thunb. var. chinense Bolle), a plant found in Southwest China, is a traditional Chinese medicine that promotes hematopoiesis and antioxidant functions. Many of its chemical constituents remain unknown, posing challenges both to understanding its pharmacological mechanisms and to conducting quality control research. In this work, ultra-high performance liquid chromatography coupled with quadrupole Exactive Orbitrap high-resolution mass spectroscopy was used for profiling the composition of Lanbuzheng. Using positive ion mass spectrometry data enriched from Lanbuzheng extract, feature-based molecular networking (FBMN) was constructed and associated with Mass2Motifs substructures using MS2LDA. Prediction and validation of unknown constituents of Lanbuzheng using a custom-built compound library, SIRIUS, and network annotation propagation, achieved a semi-automated annotation of the molecular network. Based on the custom-built library comprising 206 compounds and the FBMN clustering results, the constituents in Lanbuzheng primarily include tannins, triterpenes, flavonoids, and phenolics. Using only 65 pre-identified compounds as references, 210 unknown compounds were annotated in various polarity regions of Lanbuzheng. Results of the current work indicate that molecular networks enable the efficient annotation of compounds in complex systems, laying the groundwork for the preliminary identification of pharmacologically active constituents of Lanbuzheng.

Asunto(s)

Medicamentos Herbarios Chinos , Espectrometría de Masas , Cromatografía Líquida de Alta Presión , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/análisis , Estructura Molecular

RESUMEN

OBJECTIVE: To investigate the nutritional content of edible medicinal materials in mountainous areas of Guizhou Province and compare the comprehensive nutritional value of different varieties. METHODS: A total of 15 kinds of edible herbs were collected from Guizhou Province. According to the national standard, direct drying method, Kjeldahl nitrogen determination method, Soxhlet extraction method, high performance liquid chromatography, inductively coupled plasma mass spectrometry and other detection method were used to determine the content of general nutrients, fat soluble vitamins, minerals and ash. According to the weight ranking of nutritional indexes in principal component analysis and membership function analysis, the quality of 9 kinds of food and drug substances and 6 kinds of Chinese medicinal materials were evaluated and ranked. RESULTS: The eigenvalues of the first 4 principal components were greater than 1, and the cumulative contribution rate was 82.32%. Compared with membership function analysis, the top 5 in comprehensive evaluation were Eucommia, Epimedium and honeysuckle, all of which were food and drug substances. The contents of calcium(851.69 mg/100 g), phosphorus(270.22 mg/100 g) and potassium(1446.48 mg/100 g) were the highest. The contents of carotene(21 963.87 µg/100 g) and vitamin E(57.82 mg/100 g) were the highest in the fat-soluble vitamins of Herbimedium. The contents of various indexes of honeysuckle were relatively high. CONCLUSION: Food and pharmaceutical substances have both medicinal value and nutritional value, and the overall nutritional benefit is higher than that of Chinese medicinal materials.

Asunto(s)

Valor Nutritivo , China , Plantas Medicinales/química , Plantas Comestibles/química , Análisis de los Alimentos , Fósforo/análisis , Altitud , Medicamentos Herbarios Chinos/análisis , Minerales/análisis

RESUMEN

The development of traditional Chinese medicine(TCM) preparations as an incubator for new drugs in medical institutions has flourished, while an evaluation index system remains to be established for comprehensively assessing the development value of these prescriptions. This study established an item pool through literature research, employed the Delphi method to determine the content of evaluation indexes, and adopted the superiority chart to determine the weight of each index. Two-level evaluation index system for the development value of TCM preparations in medical institutions was established, which included 7 first-level items and 36 se-cond-level items, demonstrating scientific validity. The first-level items(weight) were inheritance(10.61%), effectiveness(23.22%), safety(22.71%), innovation(13.21%), economy(10.00%), suitability(8.57%), and accessibility(11.68%). The top three second-level items in terms of weight distribution were adverse reaction monitoring(6.73%), evidence of therapeutic effect(5.71%), and clinical response rate(4.75%). The bottom three second-level items were production advantages(0.86%), medicinal dosage(0.48%), and medicinal smell or taste(0.18%). The content validity of the established system was assessed, which revealed that the index system was reliable, with the overall and average content validity indexes of 0.47 and 0.90, respectively. Furthermore, the established evaluation index system was used to evaluate six TCM preparations in a city-level hospital of TCM in Sichuan Province, which demonstrated that the system had operability. The results indicate that the evaluation index system is scientific, reliable, and operable, providing a reference for developers to selectively develop TCM preparations in medical institutions. In practical application, the system can be adjusted regarding the index weights according to actual conditions.

Asunto(s)

Medicamentos Herbarios Chinos , Medicina Tradicional China , Medicina Tradicional China/normas , Medicamentos Herbarios Chinos/normas , Medicamentos Herbarios Chinos/análisis , Medicamentos Herbarios Chinos/química , Humanos