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1.
Zhongguo Zhong Yao Za Zhi ; 46(16): 4244-4251, 2021 Aug.
Artículo en Chino | MEDLINE | ID: mdl-34467739

RESUMEN

Coumarins are the main active components in Psoraleae Fructus. To study the multi-component pharmacokinetics of Psoraleae Fructus, this study established a sensitive and rapid ultra-pressure liquid chromatography coupled to tandem mass spectrometry(UPLC-MS/MS) method for simultaneous determination of psoralen, isopsoralen, psoralenoside, and isopsoralenoside in rat plasma. After validation, the method was applied to the investigation of pharmacokinetics of psoralen, isopsoralen, psoralenoside, and isopso-ralenoside in rats after single and multiple administration of Psoraleae Fructus extract. The results revealed that the exposure of psoralen and isopsoralen in rat plasma was high after a single intragastric administration of Psoraleae Fructus extract, with an AUC_(0-∞) of 443 619-582 680 and 167 314-276 903 ng·mL~(-1)·h~(-1), respectively. Compared with these two compounds, the exposure of psoralenoside and isopsoralenoside was lower with marked gender difference. After 7-day administration of Psoraleae Fructus extract to rats, the AUC_(0-∞) of psoralen and isopsoralen was 29 701-81 783 and 39 234-89 914 ng·mL~(-1)·h~(-1), respectively, which was significantly lower than that at the first day(P<0.05), and that of psoralenoside and isopsoralenoside was 7 360-19 342 and 8 823-45 501 ng·mL~(-1)·h~(-1), respectively. There was no significant gender difference in exposure of psoralenoside and isopsoralenoside in male and female rats. However, the exposure of psoralenoside and isopsoralenoside in male rats was reduced(P<0.05), and the t_(1/2) and mean residence time(MRT) were shortened, suggesting that the removal of these two compounds from the body was accelerated.


Asunto(s)
Medicamentos Herbarios Chinos , Furocumarinas , Psoralea , Administración Oral , Animales , Benzofuranos , Cromatografía Líquida de Alta Presión , Cromatografía Liquida , Ficusina , Furocumarinas/análisis , Glicósidos , Ratas , Espectrometría de Masas en Tándem
2.
Zhongguo Zhong Yao Za Zhi ; 46(2): 444-453, 2021 Jan.
Artículo en Chino | MEDLINE | ID: mdl-33645134

RESUMEN

An UPLC-MS/MS method for rapid and simultaneous determination of psoralen, isopsoralen, apigenin, genistein, bavaisoflavone, neobavaisoflavone, bavachin, bavachinin, psoralenoside, and isopsoralenoside of Psoraleae Fructus in beagle dog plasma was established, and then the method was applied in the pharmacokinetic study after oral administration of Psoraleae Fructus extract to beagle dogs. The pharmacokinetic parameters were calculated by the software of WinNonlin. A Waters HSS-T3 column(2.1 mm×100 mm,1.8 µm)was used for liquid chromatography separation with acetonitrile-water(containing 0.004% formic acid) as the mobile phase for gradient elution.The mass spectrometry was detected using electrospray ion source(ESI) under multi-reaction monitoring mode(MRM), as well as positive ion mode. Analysis time only takes 8.5 min. The methodological study in terms of specificity, accuracy, precision, linear range, recovery, matrix effect, and stability, was validated. The LC-MS analysis method established in this experiment was simple, specific, accurate, reliable, and meet the requirement of pharmacokinetic study in plasma after administration of Psoraleae Fructus extract to beagle dogs. Six beagle dogs received intragastric administration of Psoraleae Fructus extract, T_(max) of 10 chemical components is 1.92-5.67 h; among them, C_(max) of psoralen, isopsoralen, psoralenoside and isopsoralenoside is 383-3 613 ng·mL~(-1), and AUC_(0-∞) is 3 556-18 949 ng·h·mL~(-1), t_(1/2) is 2.45-4.83 h. C_(max) of the remaining six compounds is 0.81-19.9 ng·mL~(-1), AUC_(0-∞ )is 6.54-178 ng·h·mL~(-1), t_(1/2) is 2.95-7.29 h. The UPLC-MS/MS analysis method established in this study was proved to be accurate and sensitive that it can be applied to the pharmacokinetic study of beagle dogs after oral administration of Psoraleae Fructus extract.


Asunto(s)
Medicamentos Herbarios Chinos , Espectrometría de Masas en Tándem , Administración Oral , Animales , Cromatografía Líquida de Alta Presión , Cromatografía Liquida , Perros , Plasma , Reproducibilidad de los Resultados
3.
Zhongguo Zhong Yao Za Zhi ; 43(2): 345-352, 2018 Jan.
Artículo en Chino | MEDLINE | ID: mdl-29552854

RESUMEN

Flavonoids are the most abundant constituents and induce these the rapeutic effects against inflammation, gastrointestinal infections, cardiovascular diseases, and respiratory. Most of these flavonoids have low content in Scutellarie Radix. It was difficult to detect some minor compounds by using LC-MS method with full scan. Based on the review of flavonoids that had been extracted from Scutellariae Radix, a method with PREC-IDA-EPI technique was developed and applied to Scutellariae Radix by using UPLC-MS/MS. A total of 97 flavonoids were identified, including 29 aglycones and 68 O-glycosides. This study laid the foundation for pharmacodynamicss of Scutellariae Radix.It is believed that an individual detection scheme based on the PREC-IDA-EPI technique could be used to identify unknown compounds.


Asunto(s)
Medicamentos Herbarios Chinos/química , Flavonoides/aislamiento & purificación , Scutellaria baicalensis/química , Cromatografía Liquida , Espectrometría de Masas en Tándem
4.
Chin J Nat Med ; 15(10): 775-784, 2017 Oct.
Artículo en Inglés | MEDLINE | ID: mdl-29103463

RESUMEN

Ginkgo diterpene lactones meglumine injection (GDLI) is a commercially available product used for neuroprotection. However, the pharmacokinetic properties of the prototypes and hydrolyzed carboxylic forms of the primary components in GDLI, i.e., ginkgolide A (GA), ginkgolide B (GB), and ginkgolide K (GK), have never been fully evaluated in beagle dogs. In this work, a simple, sensitive, and reliable method based on ultra-fast liquid chromatography-tandem mass spectrometry (UFLC-MS/MS) was developed, and the prototypes and total amounts of GA, GB, and GK were determined in beagle dog plasma. The plasma concentrations of the hydrolyzed carboxylic forms were calculated by subtracting the prototype concentrations from the total lactone concentrations. For the first time, the pharmacokinetics of GA, GB, and GK were fully assessed in three forms, i.e., the prototypes, the hydrolyzed carboxylic forms, and the total amounts, after intravenous administration of GDLI in beagle dogs. It was shown that ginkgolides primarily existed in the hydrolyzed form in plasma, and the ratio of hydrolysates to prototype forms of GA and GB decreased gradually to a homeostatic ratio. All of the three forms of the three ginkgolides showed linear exposure of AUC to the dosages. GA, GB, and GK showed a constant half-life approximately 2.7, 3.4, and 1.2 h, respectively, which were consistent for the forms at three dose levels (0.3, 1.0, and 3.0 mg·kg-1) and after a consecutive injection of GDLI for 7 days (1.0 mg·kg-1).


Asunto(s)
Ginkgo biloba/química , Ginkgólidos/farmacocinética , Lactonas/farmacocinética , Extractos Vegetales/farmacocinética , Animales , Perros , Ginkgólidos/administración & dosificación , Lactonas/administración & dosificación , Extractos Vegetales/administración & dosificación , Espectrometría de Masas en Tándem
5.
J Pharm Biomed Anal ; 142: 190-200, 2017 Aug 05.
Artículo en Inglés | MEDLINE | ID: mdl-28514718

RESUMEN

Cerebral ischemia-reperfusion (I/R) injury usually contributes to mortality and disability after ischemic stroke. Ginkgolides injection (GIn), a standard preparation composed of ginkgo diterpene lactones extract, is clinically used for neuroprotective treatment on reconvalescents of cerebral infarction. However, the understanding about its therapeutic mechanism is still lacking. In this study, a gas chromatography-mass spectrometry (GC-MS) based metabolomic approach coupled with multivariate data analysis (MVDA) was applied to explore the neuroprotective effects of GIn in a rodent model of focal ischemic stroke induced by transient middle cerebral artery occlusion (tMCAO). Metabolomic profiling revealed a series of metabolic perturbations that underlie the cerebral I/R pathological events. GIn can reverse the I/R induced brain metabolic deviations by modulating multiple metabolic pathways, such as glycolysis, Krebs cycle, pentose phosphate pathway (PPP), γ-aminobutyrate (GABA) shunt and lipid metabolism. Moreover, the main bioactive components of GIn were distributed to brain tissue much more easily in tMCAO rats than in normal rats after an intravenous administration, suggesting that the increased cerebral exposure to ginkgolides in I/R pathological condition potentially facilitated the neuroprotective effects of GIn by directly targeting at brain. The present study provided valuable information for our understanding about metabolic changes of cerebral I/R injury and clinical application of GIn.


Asunto(s)
Isquemia Encefálica , Animales , Cromatografía de Gases y Espectrometría de Masas , Ginkgólidos , Infarto de la Arteria Cerebral Media , Fármacos Neuroprotectores , Ratas , Ratas Sprague-Dawley , Daño por Reperfusión
6.
Mar Biotechnol (NY) ; 18(3): 301-13, 2016 Jun.
Artículo en Inglés | MEDLINE | ID: mdl-27153822

RESUMEN

Marine sponges are ancient and simple multicellular filter-feeding invertebrates attached to solid substrates in benthic habitats and host a variety of fungi both inside and on their surface because of its unique ingestion and digest system. Investigation on marine sponge-associated fungi mainly focused on the small molecular metabolites, yet little attention had been paid to the extracellular polysaccharides. In this study, a homogeneous extracellular polysaccharide AS2-1 was obtained from the fermented broth of the marine sponge endogenous fungus Alternaria sp. SP-32 using ethanol precipitation, anion-exchange, and size-exclusion chromatography. Results of chemical and spectroscopic analyses showed that AS2-1 was composed of mannose, glucose, and galactose with a molar ratio of 1.00:0.67:0.35, and its molecular weight was 27.4 kDa. AS2-1 consists of a mannan core and a galactoglucan chain. The mannan core is composed of (1→6)-α-Manp substituted at C-2 by (1→2)-α-Manp with different degrees of polymerization. The galactoglucan chain consists of (1→6)-α-Glcp residues with (1→6)-ß-Galf residues attached to the last glucopyranose residue at C-6. (1→6)-ß-Galf residues have additional branches at C-2 consisting of disaccharide units of (1→2)-ß-Galf and (1→2)-α-Glcp residues. The glucopyranose residue of the galactoglucan chain is linked to the mannan core. AS2-1 possessed a high antioxidant activity as evaluated by scavenging of 1,1-diphenyl-2-picrylhydrazyl and hydroxyl radicals in vitro. AS2-1 was also evaluated for cytotoxic activity on Hela, HL-60, and K562 cell lines by the MTT and SRB methods. The investigation demonstrated that AS2-1 was a novel extracellular polysaccharide with different characterization from extracellular polysaccharides produced by other marine microorganisms.


Asunto(s)
Alternaria/química , Antioxidantes/química , Polisacáridos Fúngicos/química , Poríferos/microbiología , Alternaria/metabolismo , Animales , Antioxidantes/aislamiento & purificación , Antioxidantes/farmacología , Compuestos de Bifenilo/antagonistas & inhibidores , Secuencia de Carbohidratos , Supervivencia Celular/efectos de los fármacos , Fermentación , Polisacáridos Fúngicos/aislamiento & purificación , Polisacáridos Fúngicos/farmacología , Galactanos/química , Galactosa/química , Glucanos/química , Glucosa/química , Células HL-60 , Células HeLa , Humanos , Radical Hidroxilo/antagonistas & inhibidores , Células K562 , Mananos/química , Manosa/química , Peso Molecular , Picratos/antagonistas & inhibidores , Polisacáridos Bacterianos/química , Agua de Mar/microbiología , Extracción en Fase Sólida/métodos , Simbiosis/fisiología
7.
Carbohydr Polym ; 147: 272-281, 2016 08 20.
Artículo en Inglés | MEDLINE | ID: mdl-27178933

RESUMEN

An extracellular polysaccharide, N1, was obtained from the culture medium of the deep-sea fungus Aspergillus versicolor N2bc by a combination of ethanol precipitation, ion-exchange and gel filtration chromatography. N1 was a mannoglucogalactan with molecular weight of about 20.5kDa. Results of chemical and spectroscopic analyses, including Fourier-transform infrared, one- and two-dimensional nuclear magnetic resonance spectroscopy showed that the main chain of N1 consisted of →2)-α-d-Glcp-(1→, →2)-ß-d-Glcp-(1→ and →6)-ß-d-Manp-(1→ units, substituted at C-6 position of →2)-α-d-Glcp-(1→ units. The branches were composed of galactofuranose-oligosaccharides built up of →5)-ß-d-Galf-(1→, →6)-ß-d-Galf-(1→ and terminal ß-d-Galf units. At an average, there were two branching points for every five sugar residues in the backbone. N1 possessed a high in vitro antioxidant activity as evaluated by scavenging assays involving superoxide, 1,1-diphenyl-2-picrylhydrazyl, hydroxyl radicals and reducing power. The investigation revealed that N1 was a novel antioxidant polysaccharide differing from previously described extracellular polysaccharides and could be a potential antioxidant.


Asunto(s)
Aspergillus/química , Polisacáridos/química , Polisacáridos/farmacología , Antioxidantes/química , Antioxidantes/farmacología , Compuestos de Bifenilo , Espacio Extracelular/química , Modelos Moleculares , Picratos
8.
Chin J Nat Med ; 14(1): 73-80, 2016 Jan.
Artículo en Inglés | MEDLINE | ID: mdl-26850350

RESUMEN

The present study was designed to determine the relationships between the performance of ethanol precipitation and seven process parameters in the ethanol precipitation process of Re Du Ning Injections, including concentrate density, concentrate temperature, ethanol content, flow rate and stir rate in the addition of ethanol, precipitation time, and precipitation temperature. Under the experimental and simulated production conditions, a series of precipitated resultants were prepared by changing these variables one by one, and then examined by HPLC fingerprint analyses. Different from the traditional evaluation model based on single or a few constituents, the fingerprint data of every parameter fluctuation test was processed with Principal Component Analysis (PCA) to comprehensively assess the performance of ethanol precipitation. Our results showed that concentrate density, ethanol content, and precipitation time were the most important parameters that influence the recovery of active compounds in precipitation resultants. The present study would provide some reference for pharmaceutical scientists engaged in research on pharmaceutical process optimization and help pharmaceutical enterprises adapt a scientific and reasonable cost-effective approach to ensure the batch-to-batch quality consistency of the final products.


Asunto(s)
Cromatografía Líquida de Alta Presión/métodos , Medicamentos Herbarios Chinos/química , Análisis de Componente Principal , Precipitación Química , Medicamentos Herbarios Chinos/análisis , Etanol , Inyecciones
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