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1.
Phytomedicine ; 128: 155361, 2024 Jun.
Article in English | MEDLINE | ID: mdl-38552434

ABSTRACT

BACKGROUND: As a traditional Chinese herbal medicine, Schisandra chinensis exhibits various effects such as liver protection, blood sugar regulation, blood lipid regulation, immune function regulation, antidepressant activity, etc. However, because of its intricate composition, diverse origins, and medicinal effects depending on complex compound groups, there are differences in the lignan composition of S. chinensis from different origins. Therefore, it is currently difficult to evaluate the quality of medicinal materials from plants of different origins using a single qualitative quality control index. PURPOSE: This paper aims to investigate the potential relationship between the lignan components of S. chinensis from different origins and to establish stable assessment indices for determining the lignan content of S. chinensis from multiple perspectives. METHODS: In this study, we collected S. chinensis samples of seven major origins in China, and randomly sampled 6-9 batches of each origin for a total of 60 batches. The lignan content was determined by HPLC, and its distribution law of the ratio of each lignan component of S. chinensis to Schisandrol A content was analyzed. Combining network pharmacology and differential analysis between samples, the stable and effective substances used as quality markers were determined. RESULTS: There were some correlations among the lignan contents of S. chinensis, some correlations between schisandrin A and other lignans of S. chinensis could be determined. The ratio of each component to the indicator component schisandrol A was evenly distributed and reflected the lignan content of S. chinensis to some extent. Four substances (schisandrol A, schisandrol B, schisantherin A, and schisandrin C) were determined by network pharmacology combined with the analysis results of HCA, PCA and PLS-DA to further optimize the model. They displayed a strong connection with the core target, a large contribution rate to the principal components, and a stable content in each batch of samples, suggesting that these components may be the main active substances of S. chinensis lignans. Therefore, they could be used as main indicators evaluating the advantages and disadvantages of S. chinensis by examining the consistency of component proportions. CONCLUSION: This method can intuitively evaluate the content of main lignans in S. chinensis. This quality assessment model is an exploration of the multi-component comprehensive evaluation system of S. chinensis, providing a new concept for the quality evaluation system of Chinese herbal medicines.


Subject(s)
Cyclooctanes , Drugs, Chinese Herbal , Lignans , Schisandra , Schisandra/chemistry , Lignans/analysis , Drugs, Chinese Herbal/chemistry , Drugs, Chinese Herbal/analysis , Chromatography, High Pressure Liquid/methods , Cyclooctanes/analysis , China , Polycyclic Compounds/analysis , Dioxoles/analysis , Quality Control , Principal Component Analysis
2.
Chem Biodivers ; 20(6): e202300372, 2023 Jun.
Article in English | MEDLINE | ID: mdl-37145919

ABSTRACT

From the fruits of Schisandra cauliflora, five new dimethylbutyrylated dibenzocyclooctadiene lignans, named schisandracaurins A-E, were isolated using separation and chromatographic techniques. Their structures were determined by extensive analyses of HR-ESI-MS, NMR, and ECD spectra. The schisandracaurins A-E potentially inhibited NO production in LPS-activated RAW264.7 cells with their IC50 values from 21.4 to 30.3 µM.


Subject(s)
Lignans , Schisandra , Schisandra/chemistry , Lipopolysaccharides/pharmacology , Molecular Structure , Fruit/chemistry , Lignans/chemistry , Cyclooctanes/pharmacology , Cyclooctanes/analysis , Cyclooctanes/chemistry
3.
Phytomedicine ; 106: 154273, 2022 Nov.
Article in English | MEDLINE | ID: mdl-36044818

ABSTRACT

BACKGROUND: Quality control of Traditional Chinese Medicines (TCMs) has improved greatly, but there is still a lack of a convincing quality evaluation system for TCMs. Developing quality control markers of TCMs based on pharmacodynamics instead of content has been an attractive approach. However, on account of neglecting phytochemistry attributes of TCMs, part of effective markers might be short of specificity and inconvenient for detecting in production manufacture, which is adverse to control the quality of TCMs systematically. PURPOSE: To build a novel and multidimensional quality assessment approach for TCMs based on pharmacodynamics and chemical properties. METHODS: Schisandra chinensis (Turcz.) Baill (S. chinensis) was used as an example and a rat depression model was built by using a chronic unpredictable mild stress procedure. For identifying the antidepressive components of S. chinensis, we elucidated its antidepressant mechanism in first-step by using quantitative RT-PCR and immunoblotting techniques. And accordingly, correlation analysis between ingredients in vivo with target proteins and anti-inflammation experiments in vitro were carried out. On the other hand, HPLC fingerprint combinations with diverse chemometrics methods were applied to analyze 14 preparations of S. chinensis to obtain its characteristic chemical information. Finally, we ascertained the quality control markers of S. chinensis by integrating the efficacious and characteristic constituents. RESULTS: Our research indicated that S. chinensis treated depression by relieving disordered monoaminergic system and ameliorating neuroinflammation. Five effective substances (schisandrol A, schisandrin A, gomisin N, schisandrin B, and schisandrin C) were screened out according to their potential anti-depression efficacy. Besides, 21 common ingredients and 4 representative constituents of S. chinensis were identified by chemical analysis, whereas only 2 characteristic quantitative markers (schisandrol A, schisandrol B) were ultimately ascertained based on previous studies. CONCLUSION: 6 components, schisandrol A, schisandrin A, gomisin N, schisandrin B, schisandrin C, and schisandrol B, possessed efficacy, measurability, and specificity, were selected as the comprehensive markers for quality control of S. chinensis. We proposed a multidimensional strategy for identifying comprehensive quality markers for TCMs in this study.


Subject(s)
Drugs, Chinese Herbal , Lignans , Schisandra , Animals , Biomarkers , Cyclooctanes/analysis , Cyclooctanes/pharmacology , Dioxoles , Drugs, Chinese Herbal/chemistry , Drugs, Chinese Herbal/pharmacology , Lignans/analysis , Polycyclic Compounds , Rats , Schisandra/chemistry
4.
J Am Chem Soc ; 143(29): 11191-11198, 2021 07 28.
Article in English | MEDLINE | ID: mdl-34266234

ABSTRACT

We present a chemical approach to profile fatty acid uptake in single cells. We use azide-modified analogues to probe the fatty acid influx and surface-immobilized dendrimers with dibenzocyclooctyne (DBCO) groups for detection. A competition between the fatty acid probes and BHQ2-azide quencher molecules generates fluorescence signals in a concentration-dependent manner. By integrating this method onto a microfluidics-based multiplex protein analysis platform, we resolved the relationships between fatty acid influx, oncogenic signaling activities, and cell proliferation in single glioblastoma cells. We found that p70S6K and 4EBP1 differentially correlated with fatty acid uptake. We validated that cotargeting p70S6K and fatty acid metabolism synergistically inhibited cell proliferation. Our work provided the first example of studying fatty acid metabolism in the context of protein signaling at single-cell resolution and generated new insights into cancer biology.


Subject(s)
Cyclooctanes/analysis , Dendrimers/metabolism , Fatty Acids/metabolism , Glioblastoma/metabolism , Single-Cell Analysis , Azides/chemistry , Azides/metabolism , Cell Proliferation , Cyclooctanes/metabolism , Dendrimers/chemistry , Fatty Acids/chemistry , Fluorescence , Glioblastoma/pathology , Humans , Molecular Structure , Surface Properties
5.
J Ethnopharmacol ; 271: 113914, 2021 May 10.
Article in English | MEDLINE | ID: mdl-33571617

ABSTRACT

ETHNOPHARMACOLOGICAL RELEVANCE: Shengmai San (SMS) has been commonly used as a traditional Chinese medicine for the treatment of cardiovascular disorders, of which drug interactions need to be assessed for the safety concern. There is little evidence for the alterations of hepatic and intestinal drug-metabolizing enzymes after repeated SMS treatments to assess drug interactions. AIM OF THE STUDY: The studies aim to illustrate the effects of repeated treatments with SMS on cytochrome P450s (CYPs), reduced nicotinamide adenine dinucleotide (phosphate)-quinone oxidoreductase (NQO), uridine diphosphate-glucuronosyltransferase (UGT), and glutathione S-transferase (GST) using in vivo rat model. MATERIALS AND METHODS: The SMS was prepared using Schisandrae Fructus, Ginseng Radix, and Ophiopogonis Radix (OR) (1:2:2). Chromatographic analyses of decoctions were performed using ultra-performance liquid chromatography (UPLC) and LC-mass spectrometry. Sprague-Dawley rats were orally treated with the SMS and its component herbal decoctions for 2 or 3 weeks. Hepatic and intestinal enzyme activities were determined. CYP3A expression and the kinetics of intestinal nifedipine oxidation (NFO, a CYP3A marker reaction) were determined. RESULTS: Schisandrol A, schisandrin B, ginsenoside Rb1 and ophiopogonin D were identified in SMS. SMS selectively suppressed intestinal, but not hepatic, NFO activity in a dose- and time-dependent manner. Hepatic and intestinal UGT, NQO and GST activities were not affected. A 3-week SMS treatment decreased the maximal velocity of intestinal NFO by 50%, while the CYP3A protein level remained unchanged. Among SMS component herbs, the decoction of OR decreased intestinal NFO activity. CONCLUSIONS: These findings demonstrate that 3-week treatment with SMS and OR suppress intestinal, but not hepatic CYP3A function. It suggested that the potential interactions of SMS with CYP 3A drug substrates should be noticed, especially the drugs whose bioavailability depends heavily on intestinal CYP3A.


Subject(s)
Cytochrome P-450 CYP3A Inhibitors/pharmacology , Drugs, Chinese Herbal/pharmacology , Intestines/enzymology , Liver/enzymology , Animals , Biomarkers/blood , Cyclooctanes/analysis , Cytochrome P-450 CYP3A/metabolism , Cytochrome P-450 CYP3A Inhibitors/analysis , Cytochrome P-450 CYP3A Inhibitors/therapeutic use , Drug Combinations , Drugs, Chinese Herbal/analysis , Drugs, Chinese Herbal/therapeutic use , Ginsenosides/analysis , Glucuronosyltransferase/metabolism , Glutathione Transferase/metabolism , Herb-Drug Interactions , Intestines/drug effects , Lignans/analysis , Liver/drug effects , Male , Microsomes/drug effects , Microsomes/enzymology , NAD(P)H Dehydrogenase (Quinone)/metabolism , Nifedipine/metabolism , Oxidation-Reduction/drug effects , Polycyclic Compounds/analysis , Rats, Sprague-Dawley , Saponins/chemistry , Spirostans/chemistry
6.
J Chromatogr Sci ; 59(5): 452-457, 2021 Apr 21.
Article in English | MEDLINE | ID: mdl-33529316

ABSTRACT

A new selective, accurate and precise chiral high-performance liquid chromatography method for the separation of (R)-N-tert-butoxy carbonyl-piperidine-3-carboxylic acid hydrazide (RE) and its enantiomer was developed. RE is a key starting material of novel ß-lactam enhancer drug Zidebactam. Chiral resolution of more than 10 was achieved on Chiralpak IA column using mobile phase consisting of n-hexane, ethanol in the ratio of 70:30, v/v. The flow rate of the mobile phase was 1.0 mL min-1 and the column oven temperature was 30°C. Detection was carried out at 225 nm. The developed method was validated as per the International Conference on Harmonization guideline. Limit of detection and limit of quantification of the enantiomeric impurity (S)-N-tert-butoxy carbonyl-piperidine-3-carboxylic acid hydrazide (SE) was 2.5 and 7.5 µg mL-1, respectively. Mean recovery of the SE was 96.83 ± 1.4%. The effect of thermodynamic parameters on the chiral separation was evaluated.


Subject(s)
Azabicyclo Compounds , Cyclooctanes , Piperidines , Azabicyclo Compounds/analysis , Azabicyclo Compounds/chemistry , Carboxylic Acids/analysis , Carboxylic Acids/chemistry , Chromatography, High Pressure Liquid , Cyclooctanes/analysis , Cyclooctanes/chemistry , Drug Contamination , Hydrazines/analysis , Hydrazines/chemistry , Limit of Detection , Linear Models , Piperidines/analysis , Piperidines/chemistry , Reproducibility of Results , Stereoisomerism , Thermodynamics
7.
Food Chem ; 338: 127836, 2021 Feb 15.
Article in English | MEDLINE | ID: mdl-32827900

ABSTRACT

In this study, roasting was applied to enhance the volatile compound content and antioxidant activity of hot-air dried omija (Schisandra chinensis Baillon) fruit. The major volatile compounds were furfural, 1,8-cineole and terpinen-4-ol. Total volatile compound concentration in omija roasted at 150 ℃ for 15 min was approximately 4 times higher than that in hot-air dried omija. Contents of monoterpenes and sesquiterpenes in roasted omija were significantly increased, compared to that of the hot-air dried omija (P < 0.05). The contents of schizandrin in extracts of hot-air dried omija and omija roasted at 150 ℃ for 10 min were determined to be 28.9 and 106.5 mg/100 g extract, respectively. The content of gomisin A from roasted omija was about 5 times higher than that of hot-air dried omija. Through this study, it is believed that the usability of omija will be expanded.


Subject(s)
Flavonoids/analysis , Lignans/analysis , Polyphenols/analysis , Schisandra/chemistry , Volatile Organic Compounds/analysis , Cooking , Cyclooctanes/analysis , Dioxoles/analysis , Fruit/chemistry , Plant Extracts/chemistry , Polycyclic Compounds/analysis , Temperature
8.
Article in English | MEDLINE | ID: mdl-33246280

ABSTRACT

Cell membrane chromatography (CMC) is effective and widely used in drug screening, especially for the analysis of complex matrixes. However, it is time-consuming and costly given that cells or animals are employed for activity confirmation, which leads to a large amount of waste being produced if the result is negative. Stepwise frontal analysis is employed to saturate the affinity stationary phase, by using a series of low- to high-concentration solutions which resultantly form a staircase pattern. In doing so, the waste of samples, caused by the balancing process, can be avoided. In this study, stepwise frontal analysis coupled with a CMC system was performed for screening and characterizing the affinity of an active compound from wuweizi. Schizandrin A was screened and identified by α1A AR /CMC coupled with UHPLC-MS/MS. By comparing the values obtained with those related to the equilibrium dissociation constant (Kd) calculated by zonal elution, the accuracy of the stepwise frontal analysis was verified. Subsequently, the type of affinity force between Schizandrin A and α1A AR was studied by thermodynamic parameters. Moreover, schizandrin A showed an antagonistic effect on phenylephrine-induced contractions, which relax prostate muscle strips in a non-competitive antagonism manner. It has already suggested that the active compound, schizandrin A, could be used as a lead compound for the treatment of benign prostate hyperplasia (BPH) and should be further studied. Thus, the findings of this study are significant given that they could result in an online screening and affinity analysis method being utilized for the discovery of medicinal compounds as well as clarify the interaction characteristics between a drug and a receptor.


Subject(s)
Chromatography, Affinity/methods , Cyclooctanes , Lignans , Plant Extracts/chemistry , Polycyclic Compounds , Schisandra/chemistry , Adrenergic alpha-1 Receptor Antagonists/metabolism , Animals , Cell Membrane/metabolism , Chromatography, High Pressure Liquid , Cyclooctanes/analysis , Cyclooctanes/chemistry , Cyclooctanes/pharmacology , Female , Fruit/chemistry , Lignans/analysis , Lignans/chemistry , Lignans/pharmacology , Male , Polycyclic Compounds/analysis , Polycyclic Compounds/chemistry , Polycyclic Compounds/pharmacology , Prostate/drug effects , Prostatic Hyperplasia , Rabbits , Rats, Sprague-Dawley , Tandem Mass Spectrometry
9.
Article in English | MEDLINE | ID: mdl-32530783

ABSTRACT

A wide variety of plant raw materials thought to promote health are used as herbal medicines as well as foods. However, there is no legal maximum or minimum concentration limit on any herbal compound when these plant raw materials are used in processed foods. Legally, these processed foods are regulated only for harmful substances, and there is no other guarantee of their contents. Therefore, the objective of this study was to determine the concentrations of 12 herbal compounds (nodakenin, decursin, decursinol angelate, morroniside, loganin, glycyrrhizic acid, liquiritigenin, puerarin, daidzin, schisandrin, gomisin A, gomisin N) in commonly used plant raw materials, such as "Angelica Gigas root", "Cornus Fruit", "Liquorice Root", "Pueraria Root", and "Schisandra Fruit"; and also in 45 processed foods, using high-performance liquid chromatography-tandem mass spectrometry (LC-MS/MS). Method validation was performed successfully using the parameters of specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision, matrix effect, extraction recovery, and stability. The 12 herbal compounds were determined to be present in all the foods advertised as containing each ingredient, although in very low concentrations in some cases. Three solid samples labelled as 100% pure material from one herbal species also contained herbal compounds found in others, so that intentional or unintentional adulteration was suspected.


Subject(s)
Food Analysis , Fruit/chemistry , Plant Roots/chemistry , Plants, Medicinal/chemistry , Benzopyrans/analysis , Butyrates/analysis , Chromatography, Liquid , Coumarins/analysis , Cyclooctanes/analysis , Dioxoles/analysis , Flavanones/analysis , Glucosides/analysis , Glycosides/analysis , Glycyrrhizic Acid/analysis , Herbal Medicine , Iridoids/analysis , Isoflavones/analysis , Lignans/analysis , Polycyclic Compounds/analysis , Tandem Mass Spectrometry
10.
J Chromatogr A ; 1618: 460942, 2020 May 10.
Article in English | MEDLINE | ID: mdl-32057448

ABSTRACT

The fruit of Schisandra chinensis (Chinese magnolia vine), the medicinal plant well-known in Traditional Chinese Medicine, gains great popularity in the modern phytopharmacology. This phenomena is related to the wide and powerful healing properties, including supporting immune, nervous and digestive systems activity. S. chinensis is also known for its adaptogenic properties which can support the treatment of neurodegenerative disorders, particularly Alzheimer's disease. The components of S. chinensis have been analyzed mostly using chromatography, including HPLC, GC and TLC. The last technique can be easily hyphenated with biological assays performed directly on a TLC plate that is using effect directed detection. TLC-direct bioautography (TLC-DB) for acetylcholinesterase (AChE) inhibition and TLC-DB against Bacillus subtilis were performed, followed by micro-preparative separation of fractions which were subsequently subjected to LC-MS tentative identification. Additionally, screening analysis was done using both biological detection and derivatization reagents (e.g. PMA, thymol, NP-PEG). Both TLC screening and effect-directed analysis (TLC-DB followed by MS analysis) of S. chinensis fruit revealed components with biological activity, especially antibacterials (e.g. citric acid) and inhibitors of AChE (mainly dibenzocyclooctadiene lignans). AChE inhibition activities were confirmed by TLC-DB for nine standards that is: 6-O-benzoylgomisin, deoxyschisandrin, gomisin A, gomisin G, schisandrin, schisandrin C, schisanhenol, schisantherin A and schisantherin B. These lignans were further identified by LC-ESI-MS in the isolated fraction revealing AChE inhibition. Moreover three other lignans: γ-schisandrin, schisandrin B and gomisin J were tentatively identified by LC-ESI-MS.


Subject(s)
Chromatography, Thin Layer/methods , Lignans/analysis , Schisandra/chemistry , Acetylcholinesterase , Cholinesterase Inhibitors/analysis , Cholinesterase Inhibitors/chemistry , Chromatography, Liquid , Cyclooctanes/analysis , Fruit/chemistry , Lignans/chemistry , Mass Spectrometry
11.
Molecules ; 25(2)2020 Jan 08.
Article in English | MEDLINE | ID: mdl-31936367

ABSTRACT

Schisantherin A is an active ingredient originating from Schisandra chinensis (Turcz.) which has hepatoprotective and anti-oxidation activities. In this study, in vitro metabolisms investigated on rat liver microsomes (RLMs) and in vivo metabolisms explored on male Sprague Dawley rats of Schisantherin A were tested, respectively. The metabolites of Schisantherin A were identified using ultra-high-performance liquid chromatography coupled with hybrid triple quadrupole time-of-flight mass spectrometry (UHPLC-Q-TOF-MS/MS). Based on the method, 60 metabolites were successfully identified and structurally characterized including 48 phase-I and 12 phase-II metabolites. Among the metabolites, 45 metabolites were reported for the first time. Moreover, 56 and eight metabolites were detected in urine and bile and 19 metabolites were identified in rats' plasma. It demonstrated that hepatic and extra-hepatic metabolic pathways were both involved in Schisantherin A biotransformation in rats. Five in vitro metabolites were structurally characterized for the first time. The results indicated that the metabolic pathways mainly include oxidation, reduction, methylation, and conjugation with glucuronide, taurine, glucose, and glutathione groups. This study provides a practical strategy for rapidly screening and identifying metabolites, and the results provide basic data for future pharmacological and toxicology studies of Schisantherin A and other lignin ingredients.


Subject(s)
Cyclooctanes/analysis , Cyclooctanes/metabolism , Dioxoles/analysis , Dioxoles/metabolism , Drug Evaluation, Preclinical , Lignans/analysis , Lignans/metabolism , Metabolome , Tandem Mass Spectrometry , Animals , Chromatography, High Pressure Liquid , Cyclooctanes/chemistry , Dioxoles/chemistry , Ions , Lignans/chemistry , Male , Metabolic Networks and Pathways , Metabolomics , Oxidation-Reduction , Rats, Sprague-Dawley
12.
Nat Prod Res ; 34(18): 2595-2601, 2020 Sep.
Article in English | MEDLINE | ID: mdl-30623674

ABSTRACT

One new sesquiterpene (α-iso-cubebenol acetate, 8), together with 9 known compounds (1-7, 9, 10) were isolated from the stems of Schisandra chinensis (Turcz.) Baill. by repeated silica gel column chromatography. Based on the results of MS, NMR spectra and comparing with literature data, the six dibenzocyclooctadiene lignans were identified as schizandrin A to C (1-3), schizandrin (4), schisantherin A (5) and gomisin J (6), the two sesquiterpenes were identified as α-iso-cubebenol (7) and α-iso-cubebenol acetate (8), while the two triterpenic acids were identified as ganwuweizic acid (9) and kadsuric acid (10). The antifeedant activity of the 10 compounds against Tribolium castaneum adults was tested. Gomisin J (6) exhibited activity at 1500 ppm concentration with 40.3% antifeeding index percentages. As for the dibenzocyclooctene lignans (compounds 1-3, 6), the number of methylenedioxies and the position of hydroxyl groups were the main factors to affect their antifeedant activities.


Subject(s)
Cyclooctanes/chemistry , Feeding Behavior/drug effects , Lignans/chemistry , Plant Stems/chemistry , Schisandra/chemistry , Tribolium , Animals , Cyclooctanes/analysis , Cyclooctanes/isolation & purification , Dioxoles/isolation & purification , Lignans/analysis , Lignans/isolation & purification , Polycyclic Compounds/isolation & purification , Sesquiterpenes/analysis , Sesquiterpenes/isolation & purification , Structure-Activity Relationship , Tribolium/drug effects , Triterpenes/analysis , Triterpenes/isolation & purification
13.
J Chromatogr A ; 1598: 122-131, 2019 Aug 02.
Article in English | MEDLINE | ID: mdl-31047662

ABSTRACT

Traditional Chinese Medicines (TCMs) have been widely used in orient countries for thousands of years, while their inconsistent quality and therapy issues have become increasingly serious as a result of the absence of effective methods for quality control. Therefore, it is necessary to develop a novel and specific evaluation system for TCMs' quality involved with not only composition but also bioactivity. In this study, we used Schisandra chinensis (Turcz.) Baill as an example and developed a novel integrated approach involved with various chemical analysis and data processing methods to explore its quality marker (Q-marker) underlying its anti-depressive effects. First, six bioactive lignans were identified and semi-quantified in rat brain samples via high resolution mass spectrometry. Then, the bioinformation analysis showed that all the six bioactive components could modulate various diseases relative to noradrenergic, dopaminergic and serotonergic pathways. Thus, the monoaminergic metabolites contained in these three pathways were selected to screen potential biomarkers of depression treated by S. chinensis based on target metabolomics using a rapid HPLC-MS/MS method. Finally, the correlation analysis between the six components and potential biomarkers was employed to uncover the Q-markers of S. chinensis. It is suggested that schisandrol A, schisandrin A, schisandrin C and gomisin N could be determined as Q-markers for S. chinensis. Thus, the integrated approach describing here for discovering Q-markers was expected to offer an alternative quality assessment strategy of herbal medicines for the first time.


Subject(s)
Drugs, Chinese Herbal/chemistry , Drugs, Chinese Herbal/standards , Medicine, Chinese Traditional/standards , Schisandra/chemistry , Animals , Biomarkers/analysis , Biomarkers/chemistry , Chromatography, High Pressure Liquid , Cyclooctanes/analysis , Gas Chromatography-Mass Spectrometry , Lignans/analysis , Plants, Medicinal/chemistry , Polycyclic Compounds/analysis , Quality Control , Rats , Tandem Mass Spectrometry
14.
Chem Pharm Bull (Tokyo) ; 67(7): 713-716, 2019 Jul 01.
Article in English | MEDLINE | ID: mdl-31006725

ABSTRACT

A reverse phase (RP)-HPLC method for separation and determination of Schisandrin A and Schisandrin B was presented, using a C18 Bondclone column, with methanol-water (v/v = 68 : 32) as mobile phase at a flow-rate of 1.00 mL·min-1, and UV detection at 220 nm. The tested parameters included mobile phase composition and UV detection wavelength. Good linearities were observed within concentration ranges of Schisandrin A 0.008-4.8 mg·L-1 (r = 0.9996), and Schisandrin B 0.005-3.1 mg·L-1 (r = 0.9994), respectively. The limit of detection (LOD) (S/N = 3) were 0.005 mg·L-1 Schisandrin A and 0.002 mg·L-1 Schisandrin B, respectively. The method was applied to determine the 2 compounds in a traditional Chinese medicine preparation for treatment of hepatic diseases, Huganpian tablet. To eliminate matrix effect, Oasis hydrophilic lipophilic balance (HLB) solid-phase extraction (SPE) was used to purify the ultra-sonicately extracted solution of the drug sample. Combined with the HLB SPE purification procedure, the HPLC method gave satisfactory results for quantitation of Schisandrin A and Schisandrin B in 3 types of Huganpian tablet samples, with spiking recoveries ca. 98% (relative standard deviation (R.S.D.) ≤ 3.5%) (n = 5).


Subject(s)
Chromatography, High Pressure Liquid , Cyclooctanes/analysis , Lignans/analysis , Polycyclic Compounds/analysis , Tablets/chemistry , Chromatography, Reverse-Phase , Cyclooctanes/isolation & purification , Lignans/isolation & purification , Limit of Detection , Medicine, Chinese Traditional , Polycyclic Compounds/isolation & purification , Solid Phase Extraction
15.
Phytomedicine ; 53: 182-192, 2019 Feb.
Article in English | MEDLINE | ID: mdl-30668398

ABSTRACT

BACKGROUND: Herbal medicines (HMs) have been proven to be productive sources of leads for the development of drugs. To date approximately 150 lignans have been identified from Schisandra sphenanthera. Hepatoprotective activity is a well-known characteristic of schisandra lignans, yet the authentic types of active lignans are still not well known. PURPOSE: The present study aimed to develop a reliable and efficient strategy for identifying the hepatoprotective ingredients of schisandra lignan extract (SLE). METHODS: SLEs were prepared by extracting Schisandra sphenanthera powder using 10%, 50% and 90% ethanol (w/w 1:10) combining 5-fold volume of ethyl acetate. The schisandra lignans in SLEs were qualitatively analyzed based on liquid chromatography hybrid ion trap time-of-flight mass spectrometry (LCMS-IT-TOF). Preparative liquid chromatography (PLC) was used to collect ingredient fractions. The hepatoprotective activity of schisandra lignans was systematically investigated on in vivo and in vitro models. RESULTS: The SLE extracted by 50% ethanol and 5-fold volume of ethyl acetate (50%SLE) had the highest lignan content and exhibited significantly stronger hepatoprotective activity than other SLEs (P <  0.01). The hepatoprotective effect of 50%SLE mainly attributed to the SLE segment which collected from 12 to 22 min by PLC. Schisantherin A (Sth A) was confirmed as the most promising hepatoprotective drug in Schisandra sphenanthera due to high content in crude materials, high exposure level in vivo and high efficiency on APAP-induced hepatotoxicity. CONCLUSION: The hepatoprotective ingredients of SLEs were systematically investigated based on the presently developed approach, and Sth A was identified as the optimum hepatoprotective candidate in Schisandra sphenanthera.


Subject(s)
Drug Evaluation, Preclinical/methods , Liver/drug effects , Plant Extracts/pharmacokinetics , Protective Agents/pharmacokinetics , Schisandra/chemistry , Animals , Chemical and Drug Induced Liver Injury/prevention & control , Chromatography, Liquid/methods , Cyclooctanes/analysis , Dioxoles/analysis , Lignans/analysis , Lignans/pharmacokinetics , Male , Mass Spectrometry/methods , Mice, Inbred BALB C , Plant Extracts/chemistry , Protective Agents/chemistry , Rats, Sprague-Dawley
16.
J Food Drug Anal ; 27(1): 284-294, 2019 01.
Article in English | MEDLINE | ID: mdl-30648582

ABSTRACT

The traditional Chinese herbal formula Shenmai-Yin (SY) and nifedipine have both been used to treat patients with cardiovascular disorders. Nifedipine is primarily oxidized by cytochrome P450 (CYP) 3A. The oxidation and pharmacokinetics of nifedipine were studied in rats in vitro and in vivo to illustrate the interaction of SY with nifedipine. Schisandrol A, schisandrin A and schisandrin B were identified as the main lignans in SY. In the study in vitro, the ethanolic extract of SY was used due to the solubility and the extract inhibited nifedipine oxidation (NFO) activity in a time-dependent manner. Among lignans, schisandrin B caused the most potent inhibition. According to the time-dependent inhibition behavior, rats were treated with SY 1 h before nifedipine administration. After oral treatment with 1.9 g/kg SY, nifedipine clearance decreased by 34% and half-life increased by 142%. SY treatment decreased hepatic NFO activity by 49%. Compared to the change caused by ketoconazole, the SY-mediated reduction of nifedipine clearance was moderate. These findings demonstrate that SY causes a time-dependent inhibition of NFO and schisandrin B contributes to the inhibition. The decreased nifedipine clearance by SY in rats warrants further human study to examine the clinical impact of this decrease.


Subject(s)
Drugs, Chinese Herbal/administration & dosage , Nifedipine/pharmacokinetics , Animals , Cyclooctanes/administration & dosage , Cyclooctanes/analysis , Cytochrome P-450 CYP3A/metabolism , Drug Interactions , Drugs, Chinese Herbal/analysis , Humans , Lignans/administration & dosage , Lignans/analysis , Male , Nifedipine/administration & dosage , Polycyclic Compounds/administration & dosage , Polycyclic Compounds/analysis , Rats , Rats, Sprague-Dawley
17.
J Nat Med ; 73(2): 381-387, 2019 Mar.
Article in English | MEDLINE | ID: mdl-30535786

ABSTRACT

Arboreous fruit of Schisandra chinensis Baillon, Schisandra Fruit (SF), is a crude drug used in Japanese traditional Kampo medicine. The marker compounds of SF for quality control are lignans, such as schizandrin (Sz) and gomisin A (GmA). Kampo formulation containing SF is usually prepared as decoctions in the dosage form of whole crude drug (W), as its size is small enough to measure using a spoon. However, in some traditional books, it has been described that SF must be used in the dosage form of crushed or cut pieces (Cr). In this study, we evaluated the transferring ratio of lignans from SF to the decoction, and the stability and taste of the decoctions of shoseiryuto (SST) and ninjin'yoeito (NYT) using each dosage form, i.e., Cr and W, of SF. The transferring ratio of Sz and GmA was significantly higher in the decoction prepared with the Cr form than that prepared using the W form in both SST and NYT. The concentration of Sz and GmA in the decoctions was stable when maintained at 4 °C for 35 days. The taste of SST decoction prepared using the Cr form was more acidic, harsher, and bitterer than SST decoction prepared using the W form, and the taste of NYT decoction prepared using the Cr form was harsher than NYT decoction prepared using the W form. In conclusion, when SF is used in Kampo prescription, crushing the fruits and seeds can increase its effectiveness.


Subject(s)
Cyclooctanes/analysis , Dioxoles/analysis , Drugs, Chinese Herbal/chemistry , Lignans/analysis , Polycyclic Compounds/analysis , Schisandra/chemistry , Adult , Female , Fruit/chemistry , Humans , Male , Medicine, Kampo , Taste , Young Adult
18.
Se Pu ; 36(8): 766-771, 2018 Aug 08.
Article in Chinese | MEDLINE | ID: mdl-30251500

ABSTRACT

The double qualitative principle is a new composite qualitative method based on retention time and the characteristic peaks of the absorption spectra. Using a self-designed and assembled diode array detector (DAD), a high performance liquid chromatography (HPLC) system was constructed. The illegal additive auramine O in six kinds of herbal slices and the active ingredient schisandrin in Jujube kernel Tianma capsules were separated and qualitative analyzed using the HPLC-DAD system. The results showed that there were similar peaks in the chromatograms of pollen typhae and Jujube kernel Tianma capsules when comparing the target analytes. However, the probabilities of the targets were excluded by comparing the absorption spectra. The application results indicated that, based on the double qualitative principle of retention time/absorption spectrum, the interference of impurities in the samples could be well eliminated and the false positives could be avoided. This provides a reference method for the study of traditional Chinese medicine components.


Subject(s)
Chromatography, High Pressure Liquid , Cyclooctanes/analysis , Drugs, Chinese Herbal/analysis , Lignans/analysis , Polycyclic Compounds/analysis
19.
Phytomedicine ; 45: 84-92, 2018 Jun 01.
Article in English | MEDLINE | ID: mdl-29685366

ABSTRACT

BACKGROUND: Shengmai San (SMS), a Chinese classic herbal formula, has been widely used for the treatment of Qi-Yin deficiency syndrome in Asia. Modern pharmacological studies have shown that SMS improves the cognitive function. However, the quality markers (Q-markers) for SMS still need further research. PURPOSE: Using chinmedocmics strategy to systematically evaluate the efficacy of SMS in the treatment of APPswe/PS1dE9 (APP/PS1) transgenic model of Alzheimer's disease (AD) and to discover the efficacy-related Q-markers. METHODS: The effect of SMS on APP/PS1 mice was evaluated by behavioral test, immunohistochemistry and urine metabolic profile, and the urine marker metabolites associated with SMS treatment of AD were characterized using metabolomics method. In the premise of efficacy, Serum Pharmacochemistry of Traditional Chinese Medicine was applied to investigate the in vivo constituents of SMS. A correlation analysis between marker metabolites of therapeutic effects and serum constituents was completed by chinmedomics approach. RESULTS: SMS had a therapeutic effect on APP/PS1 mice, and 34 potential urine biomarkers were reversed by SMS treatment. A total of 17 in vivo constituents were detected, including 14 prototype components and 3 metabolites. The correlation analysis showed that eight constituents were extremely correlated with protective effects of SMS in AD, and considered as potential Q-markers of SMS, including schisandrin, isoschisandrin, angeloylgomisin Q, gomisin D, angeloylgomisin H, gomisin M2, ginsenoside F1, 20(R)-ginsenoside Rg3. CONCLUSION: This study has demonstrated that chinmedomics is novel strategy for discovering the potential effective constituents from herbal formula, which are recognized as Q-markers.


Subject(s)
Alzheimer Disease/drug therapy , Biomarkers, Pharmacological/analysis , Drugs, Chinese Herbal/chemistry , Drugs, Chinese Herbal/pharmacology , Animals , Biomarkers, Pharmacological/blood , Biomarkers, Pharmacological/urine , Cyclooctanes/analysis , Dioxoles/analysis , Disease Models, Animal , Drug Combinations , Drugs, Chinese Herbal/analysis , Ginsenosides/analysis , Lignans/analysis , Male , Medicine, Chinese Traditional/methods , Metabolomics/methods , Mice, Transgenic , Neuroprotective Agents/chemistry , Neuroprotective Agents/pharmacology , Polycyclic Compounds/analysis
20.
Chin J Nat Med ; 16(12): 916-925, 2018 Dec.
Article in English | MEDLINE | ID: mdl-30595216

ABSTRACT

Schisandra chinensis, a traditional Chinese medicine (TCM), has been used to treat sleep disorders. Zebrafish sleep/wake behavioral profiling provides a high-throughput platform to screen chemicals, but has never been used to study extracts and components from TCM. In the present study, the ethanol extract of Schisandra chinensis and its two main lignin components, schisandrin and schisandrin B, were studied in zebrafish. We found that the ethanol extract had bidirectional improvement in rest and activity in zebrafish. Schisandrin and schisandrin B were both sedative and active components. We predicted that schisandrin was related to serotonin pathway and the enthanol extract of Schisandra chinensis was related to seoronin and domapine pathways using a database of zebrafish behaviors. These predictions were confirmed in experiments using Caenorhabditis elegans. In conclusion, zebrafish behavior profiling could be used as a high-throughput platform to screen neuroactive effects and predict molecular pathways of extracts and components from TCM.


Subject(s)
Behavior, Animal/drug effects , Central Nervous System Agents/pharmacology , Drugs, Chinese Herbal/pharmacology , Plant Extracts/pharmacology , Schisandra/chemistry , Zebrafish/physiology , Animals , Caenorhabditis elegans , Central Nervous System Agents/chemistry , Central Nervous System Agents/isolation & purification , Cyclooctanes/analysis , Cyclooctanes/isolation & purification , Cyclooctanes/pharmacology , Drugs, Chinese Herbal/chemistry , Lignans/analysis , Lignans/isolation & purification , Lignans/pharmacology , Plant Extracts/chemistry , Plant Extracts/isolation & purification , Polycyclic Compounds/analysis , Polycyclic Compounds/isolation & purification , Polycyclic Compounds/pharmacology
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