RESUMEN
Ginkgo diterpene lactone (GDL) is the raw material for ginkgo diterpene lactone meglumine injection, which is used for treating cerebral ischemia. The aims of this study were to explore the cellular pharmacokinetics of GDL in whole cells and subcellular fractions, and detect cellular pharmacodynamics on the human SH-SY5Y cells induced by oxygen-glucose deprivation and reoxygenation (OGD/R). Firstly, a simple, sensitive and reliable liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for assessing the amount of ginkgolide A (GA), B (GB) and K (GK) in cellular/subcellular samples. Then, phosphatidylserine and mitochondria membrane potential were assayed to evaluate the extent of apoptosis effect. The study showed that the cellular/subcellular accumulation of GA and GB were increased in a concentration-dependent manner; the levels of GA and GB in cytosol were the highest among these subcellular organelles. Meanwhile, GDL also attenuated the OGD/R-induced increases in the percentage of apoptotic and mitochondria membrane potential. In addition, verapamil increased the rate and amount of GA and GB entering cellular/subcellular compartments through inhibition of P-glycoprotein activity, and promoted the protective effect of GDL. The present study reports the cellular pharmacokinetics profiles of GA and GB in normal and OGD/R-induced SH-SY5Y cells in vitro for the first time, which provided valuable information for clinical safety application.
Asunto(s)
Miembro 1 de la Subfamilia B de Casetes de Unión a ATP , Diterpenos , Ginkgo biloba/química , Lactonas , Miembro 1 de la Subfamilia B de Casetes de Unión a ATP/antagonistas & inhibidores , Miembro 1 de la Subfamilia B de Casetes de Unión a ATP/metabolismo , Línea Celular Tumoral , Supervivencia Celular/efectos de los fármacos , Cromatografía Liquida , Diterpenos/química , Diterpenos/farmacocinética , Diterpenos/farmacología , Humanos , Lactonas/química , Lactonas/farmacocinética , Lactonas/farmacología , Límite de Detección , Modelos Lineales , Potencial de la Membrana Mitocondrial/efectos de los fármacos , Extractos Vegetales/química , Reproducibilidad de los Resultados , Espectrometría de Masas en TándemRESUMEN
As an important integral part of traditional Chinese medicine chemical biology( TCMCB),it is of great importance to rapid isolate,and reliably identify the chemical components in herbal medicines. Phytochemical studies on the anti-inflammatory active part of Chinese dragon's blood,the red resin of Dracaena cochinchinensis,resulted in the isolation of two compounds,nordracophane( 1) and dracophane( 2),using LC-MS and chromatographic techniques( Silica gel,ODS and preparative HPLC). The structures,cyclic dihydrochalcane trimers,were elucidated on the basis of 1 D and 2 D NMR,MS,IR and UV spectral analysis. Compound 1 is a new compound,and 2 is isolated from D. cochinchinensis for the first time. Both compounds exhibited significant inhibition of nitric oxide production in lipopolysaccharides( LPS)-stimulated RAW264. 7 cells with IC50 values of( 14. 9±4. 50) and( 9. 0±0. 7) µmol·L-1.
Asunto(s)
Antiinflamatorios/aislamiento & purificación , Espectrometría de Masas , Extractos Vegetales/aislamiento & purificación , Animales , Cromatografía Liquida , Dracaena , Ratones , Óxido Nítrico/metabolismo , Células RAW 264.7RESUMEN
The study aims to qualitatively analyze the chemical composition of compound Nanxing acesodyne plaster by ultra-high performance liquid chromatography-quadrupole time-of-flight mass spectrometry( UPLC-Q-TOF-MS/MS). The analysis was performed on Agilent Zorbax SB-C_(18)( 4. 6 mm×250 mm,5 µm) column. The mobile phase consisted of methanol and 0. 2% formic acid-water was used as gradient elution. The flow rate was 1 mL·min~(-1) and column temperature was 30 â. The Mass spectrometry was acquired in both positive and negative ion modes using ESI. The components were identified by the precise mass-to-charge ratio,secondary fragmentation and other information combined with reference substance and literature data. As a result,58 compounds were identified and predicted,including alkaloids,flavonoids,coumarins,organic acids and lactone compounds,of which 12 compounds were verified by the reference substances. The results provide reference for the quality control of compound Nanxing acesodyne plaster,and lay the foundation for elucidating the active components mechanism.
Asunto(s)
Cromatografía Líquida de Alta Presión , Medicamentos Herbarios Chinos/química , Fitoquímicos/análisis , Espectrometría de Masas en TándemRESUMEN
Ten fractions(A-J) were prepared by separation of Longxue Tongluo Capsules(LTC) by using silica gel column chromatography and orthogonal experimental design,showing similar chemical profiles with different abundances of peaks.These ten samples were assessed with UHPLC-QE OrbitrapHRMS for 97 common peaks.For the pharmacological activity experiment,three kinds of in vitro cell models including lipopolysaccharide(LPS)-induced BV-2 microglial cells NO release model,oxygen-glucose deprivation/reoxygenation(OGD/R)-treated HUVEC vascular endothelial cells injury model,and OGD/R-treated PC-12 nerve cells injury model were employed to evaluated the bioactivity of each fraction.Based on the contribution of each identified component,grey relation analysis and partial least squares(PLS) analysis were performed to establish component-activity relationship of LTC,identify the potential active components.After that,validation of the potential active components in LTC was carried out by using the same models.The results indicated that 4 phenolic compounds including 7,4'-dihydroxyhomoisoflavanone,loureirin C,4,4'-dihydroxy-2,6-dimethoxydihydrochalcone,and homoisosocotrin-4'-ol,might be the active components for anti-neuroinflammation effect;five phenolic compounds such as 3,5,7,4'-tetrahydroxyhomoisoflavanone,loureirin D,7,4'-dihydroxyhomoisoflavane,and 5,7-dihydroxy-4'-methoxy-8-methyflavane,might have positive effects on the vascular endothelial injury;three phenolic compounds including 5,7,4'-trihydroxyflavanone,7,4'-dihydroxy-5-methoxyhomoisoflavane,and loureirin D,might be the active components in LTC against neuronal injury.
Asunto(s)
Isquemia Encefálica/tratamiento farmacológico , Medicamentos Herbarios Chinos/farmacología , Células Endoteliales de la Vena Umbilical Humana/efectos de los fármacos , Microglía/efectos de los fármacos , Cápsulas , Línea Celular , Glucosa , Humanos , OxígenoRESUMEN
ETHNOPHARMACOLOGICAL RELEVANCE: Gardenia jasminoides fruit (GJF) is used as a well-known traditional folk medicine, a food and a natural colorant in Asia with a long history. The herbal medicine has usually been harvested in the autumn from September to November. However, this time span is too long and might result in the quality instability of GJF. AIM OF STUDY: We aimed to conduct the comprehensive quality evaluation of GJF including the quantitative analysis of the bioactive components and the main bioactivities, and further to determine the most appropriate harvest time of this phytomedicine. MATERIALS AND METHODS: In this study, an UFLC-Q-TRAP-MS/MS method was established to quantify 7 iridoid glycosides (geniposide, geniposidic acid, secoxyloganin, gardenoside, genipin 1-gentiobioside, scandoside methyl ester, and shanzhiside), 7 phenylpropanoid acids (chlorogenic acid, cryptochlorogenic acid, neochlorogenic acid, isochlorogenic acid A, isochlorogenic acid B, isochlorogenic acid C, and caffeic acid) and 2 carotenoids (crocin-1 and crocin-2) in GJF. With this method, nine samples of GJF harvested at different times were analyzed and compared. These samples were also investigated and compared in terms of their antioxidant activity (DPPH free radical scavenging, ABTS free radical scavenging, ferric-reducing antioxidation) and anti-influenza activity (neuraminidase inhibition), which are closely related to the GJF efficacies. Then, hierarchical cluster analysis (HCA) was separately performed for the quantitative analysis and bioactivity evaluation in vitro. RESULTS: The HCA results demonstrated that three GJF samples (S5, S6, and S7) were clustered into one group for both quantitative analysis and bioactivity evaluation in vitro; these three samples were found to have the highest standardized scores in both the former (12.775, 12.106, 10.817) and the latter (3.406, 3.374, 3.440). Based on the comprehensive results, the optimum harvest period was confirmed to extend from mid-October to early-November. CONCLUSIONS: This study firstly validated the use of UFLC-Q-TRAP-MS/MS method for the determination of 16 bioactive components in GJF. It was also the first time that a quantitative analysis and a bioactivity assay in vitro were integrated for the determination of the most appropriate harvest period of GJF. We hope this paper may provide some reference to studies of appropriate harvest periods and even the quality control of TCMs.
Asunto(s)
Antioxidantes , Antivirales , Gardenia , Fitoquímicos , Agricultura/métodos , Antioxidantes/química , Antivirales/química , Benzotiazoles/química , Compuestos de Bifenilo/química , Análisis por Conglomerados , Frutas/química , Gardenia/química , Neuraminidasa/antagonistas & inhibidores , Fitoquímicos/análisis , Picratos/química , Ácidos Sulfónicos/químicaRESUMEN
A new dimeric secoiridoids derivative, named japonicaside E, together with six known compounds were isolated from the flower buds of Lonicera japonica. The structures of these compounds were elucidated by the analyses of mass spectrometry and NMR spectroscopy. All compounds were evaluated for anti-inflammatory activity in vitro.
Asunto(s)
Iridoides/aislamiento & purificación , Lonicera/química , Antiinflamatorios/aislamiento & purificación , Antiinflamatorios/farmacología , Flores/química , Espectroscopía de Resonancia Magnética , Espectrometría de Masas , Estructura MolecularRESUMEN
Two new labdane diterpenoids, Leojaponin E (1) and F (2), together with three known compounds were isolated from the dried herb of Leonurus japonicus Houtt., Lamiaceae. Their structures were determined based on extensive spectroscopic analyses. The absolute configurations of 1 and 2 were elucidated on the basis of experimental and calculated electronic circular dichroism spectra. In addition, compounds 1 and 2 exerted inhibition of LPS-induced PGE2 production in a dose-dependent manner at concentrations ranging from 5 to 20 µM.
Asunto(s)
Antiinflamatorios no Esteroideos/farmacología , Diterpenos/química , Diterpenos/farmacología , Leonurus/química , Animales , Antiinflamatorios no Esteroideos/administración & dosificación , Antiinflamatorios no Esteroideos/química , Dicroismo Circular , Dinoprostona/biosíntesis , Relación Dosis-Respuesta a Droga , Evaluación Preclínica de Medicamentos , Lipopolisacáridos/farmacología , Espectroscopía de Resonancia Magnética , Ratones , Estructura Molecular , Componentes Aéreos de las Plantas/química , Células RAW 264.7RESUMEN
To analyze and identify the chemical components in Xingbei Zhike Keli by using ultra-performance liquid chromatography-quadrupole-time of flight mass spectrometry (UPLC-Q-TOF-MS/MS). The analysis was performed on Agilent Zorbax SB-C18(4.6 mm×250 mm, 5 µm) column, with methanol-0.08% formic acid solution (including 0.1% ammonium formate) as the mobile phase for gradient elution. The flow rate was 1 mL·min⻹ and column temperature was 30 °C. The MS spectrum was acquired in both negative and positive ion modes by using electron spray ionization (ESI). These components were further analyzed based on accurate m/z, secondary fragmentation and other information combined with reference substance and literature data. As a result, 87 compounds were successfully identified and predicted, including alkaloids, flavonoids, coumarins and saponins, of which 23 compounds were verified by comparing with reference substances. These results provide reference for the quality control of Xingbei Zhike Keli, and lay the foundation for elucidating their effective components and mechanism of action.
Asunto(s)
Medicamentos Herbarios Chinos , Alcaloides , Cromatografía Líquida de Alta Presión , Flavonoides , Espectrometría de Masa por Ionización de Electrospray , Espectrometría de Masas en TándemRESUMEN
The qualitative analysis method of RRLC-Q-TOF-MS/MS was established for determine the chemical constituents in Qige Keli. Kramosil C18 column (4.6 mm×150 mm, 3.5 µm) was used at the temperature of 30 °C. The mobile phase was 0.2% formic acid and acetonitrile by gradient elution, with a flow rate at 1.0 mL·min⻹, and the injection volume was 10 µL. The high-resolution quadrupole time-flight mass spectrometry was used as detector with electrospray ion source in both positive and negative models. On the basis of medicinal materials, reference materials, literature reports, and mass spectrometry data, the chemical composition in the Qige Keli was identified. A total of 44 compounds were identified, including 3 flavonoids, 21 flavonoid glycosides, 8 organic acids, 6 lactones, and 3 saponins. The results laid the foundation for the quality control of Qige Keli and the further research on pharmacodynamic materials.
Asunto(s)
Medicamentos Herbarios Chinos/química , Fitoquímicos/análisis , Ácidos/análisis , Flavonoides/análisis , Glicósidos/análisis , Lactonas/análisis , Saponinas/análisis , Espectrometría de Masa por Ionización de Electrospray , Espectrometría de Masas en TándemRESUMEN
Five new homoisoflavonoid derivatives, including three meta-homoisoflavanes (1-3), one homoisoflavanone (4), and one homoisoflavan (5), along with five known analogues (6-10), were isolated from the red resin of Dracaena cochinchinensis (Chinese dragon's blood). Their structures were elucidated by analysis of spectroscopic data (1D and 2D NMR, IR, and HRESIMS). The absolute configuration of compound 1 was determined by single-crystal X-ray crystallographic analysis, and those of 2-5 were established on the basis of experimental and computed ECD data. Compounds 4, 6, and 9 exhibited moderate inhibition of nitric oxide production in lipopolysaccharide-stimulated BV-2 microglial cells with IC50 values of 60.4-75.6⯵M.
Asunto(s)
Dracaena/química , Isoflavonas/aislamiento & purificación , Resinas de Plantas/química , Animales , Línea Celular , Cristalografía por Rayos X , Ratones , Microglía/efectos de los fármacos , Estructura Molecular , Óxido Nítrico/metabolismo , Fitoquímicos/aislamiento & purificación , Extractos Vegetales/químicaRESUMEN
Focal cerebral ischemia reperfusion is an essential process during ischemic stroke. The apoptosis of vascular endothelial cells induced by ischemia/reperfusion (I/R) injury is an important cause for brain injury after focal cerebral ischemia. Longxuetongluo capsule (LTC) has been used for the treatment of ischemic stroke in clinic. However, its underlying action mechanism is still unclear. This study aimed to verify the protective effect and mechanisms of LTC on HUVEC cells against oxygen-glucose deprivation/reoxygenation (OGD/R) injury through MTT, LDH, flow cytometry, AO/EB staining and western blot assays. As a result, OGD/R significantly decreased the viability of HUVEC cells, which was significantly improved by LTC. LDH release assay showed that OGD/R significantly increased the lactate dehydrogenase (LDH) release, and LTC dramatically reduced the OGD/R-induced LDH release. Further mechanism study indicated that LTC dose-dependently inhibited the cleavage of PARP, caspase 3, and caspase 9 induced by OGD/R, suggesting that LTC could inhibit the activation of caspase 3/9 apoptosis pathway in the OGD/R-induced apoptosis of HUVEC cells. In conclusion, LTC could protect HUVEC cells against OGD/R injury by inhibiting the activation of mitochondria-related caspase 3/9 apoptosis pathway.
Asunto(s)
Apoptosis/efectos de los fármacos , Medicamentos Herbarios Chinos/farmacología , Células Endoteliales/efectos de los fármacos , Daño por Reperfusión , Supervivencia Celular , Glucosa , Humanos , OxígenoRESUMEN
Analysis errors can occur in the desorbing process of ginkgo diterpene lactone meglumine injection (GDMI) by a conventional analysis method, due to several factors, such as easily crystallized samples, solvent volatility, time-consuming sample pre-processing, fixed method, and offline analysis. Based on risk management, near-infrared (NIR) and mid-infrared (MIR) spectroscopy techniques were introduced to solve the above problems with the advantage of timely analysis and non-destructive nature towards samples. The objective of the present study was to identify the feasibility of using NIR or MIR spectroscopy techniques to increase the analysis accuracy of samples from the desorbing process of GDMI. Quantitative models of NIR and MIR were established based on partial least square method and the performances were calculated. Compared to NIR model, MIR model showed greater accuracy and applicability for the analysis of the GDMI desorbing solutions. The relative errors of the concentrations of Ginkgolide A (GA) and Ginkgolide B (GB) were 2.40% and 2.89%, respectively, which were less than 5.00%. The research demonstrated the potential of the MIR spectroscopy technique for the rapid and non-destructive quantitative analysis of the concentrations of GA and GB.
Asunto(s)
Química Farmacéutica/métodos , Ginkgólidos/análisis , Meglumina/análisis , Gestión de Riesgos , Espectrofotometría Infrarroja/normas , Química Farmacéutica/normas , Composición de Medicamentos/normas , Medicamentos Herbarios Chinos/análisis , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/normas , Ginkgólidos/química , Ginkgólidos/normas , Inyecciones , Lactonas/análisis , Análisis de los Mínimos Cuadrados , Meglumina/química , Meglumina/normas , Reproducibilidad de los ResultadosRESUMEN
Platelet activating factor(PAF), an endogenous synthesized phospholipid transmitter, has widely biological activities. It has "signal transmission" effect in various life processes, but abnormality of concentration in vivo will promote or aggravate the diseases, such as, cerebral ischemia, myocardial injury, multi-organ failure, asthma, injury of liver and kidney, severely affecting the normal life activities of body. In recent years, with the development of medical science and technology, more and more attention has been paid to the research of platelet activating factor receptor antagonist. Components of animals, plants, microbial fermentation, and synthetic composition all can reflect such activity. Ginkgolide B and cytopone are the most representative herbal compositions at present. This paper referred to the research status of platelet activating factor receptor antagonist in recent years, made a summary of the researches on biological effect of platelet activating factor and platelet receptor antagonist of different sources, so as to provide a reference for the exploration of effective and safe platelet activating factor receptor antagonists.
Asunto(s)
Factor de Activación Plaquetaria , Glicoproteínas de Membrana Plaquetaria/antagonistas & inhibidores , Receptores Acoplados a Proteínas G/antagonistas & inhibidores , Animales , Humanos , PlantasRESUMEN
Ginkgo diterpene lactone raw material, as a raw material for ginkgo diterpene lactone meglumine injection, is extracted and purified from ginkgo leaf. ¹H-NMR content determination method and fingerprint analysis method were respectively established for ginkgo diterpene lactone raw material. Content determination was conducted in 3 batches of samples by using ¹H-qNMR, and then the results were basically consistent with the results in HPLC method. Twenty-four proton peaks were identified as common fingerprint peaks, and the fingerprint peaks were identified by using the control product and NMR information. Furthermore, 10 batches of samples were analyzed by ¹H-NMR fingerprint. The similarities were all higher than 0.99 and the common peaks were identified with the reference standards. This method is easy, fast, with good precision, stability and repeatability and could provide basis and new ideas for quality evaluation of ginkgo diterpene lactone raw material and its preparations.
Asunto(s)
Diterpenos/análisis , Ginkgo biloba/química , Lactonas/análisis , Cromatografía Líquida de Alta Presión , Medicamentos Herbarios Chinos/análisis , Espectroscopía de Protones por Resonancia Magnética , Control de CalidadRESUMEN
Ginkgo terpene lactones, as an important active ingredient from Ginkgo leaves, has high medicinal values and has been widely used in clinics. This article would review the researches both at home and abroad, including chemical composition, structure-activity relationship, analytical methods, pharmacological effects, pharmacokinetic characteristics, and so on, providing a reference for further development and utilization of ginkgo terpene lactones.
Asunto(s)
Ginkgo biloba/química , Lactonas/química , Hojas de la Planta/química , Terpenos/química , Medicamentos Herbarios Chinos/química , Medicamentos Herbarios Chinos/farmacología , Lactonas/farmacología , Terpenos/farmacologíaRESUMEN
A new compound(Z)-6-hydroxy-4-methoxy-5,7-dimethylaurone was isolated from Cleistocalyx operculatus flower buds. Its structure was identified by spectroscopic data including MS, ¹H-NMR, ¹³C-NMR HSQC and HMBC. A known compound, 2',4'-dihydroxy-6'-methoxy-3'5'-dimethylchalcone (DMC), was also isolated and identified,and used as material to synthesize (Z)-6-hydroxy-4-methoxy-5,7-dimethylaurone.Anti-inflammatory activities of the two compounds were tested in vitro. The results showed that (Z)-6-hydroxy-4-methoxy-5,7-dimethylaurone possesses much stronger PGE2 inhibitory activity (IC50 6.12 nmol·L⻹) than the positive control ibuprofen ï¼68.66 nmol·L⻹ï¼.
Asunto(s)
Antiinflamatorios/farmacología , Benzofuranos/farmacología , Flores/química , Syzygium/química , Antiinflamatorios/aislamiento & purificación , Benzofuranos/aislamiento & purificación , Chalconas , Dinoprostona/antagonistas & inhibidoresRESUMEN
To observe the protective effect of Longxue Tongluo capsule (LTC) on human umbilical vein endothelial cells (EAhy.926 cells) injury induced by oxidized low-density lipoprotein (ox-LDL, 100 mg·L⻹). The effect of the cell viability of LTCin alleviating OX-LDL-induced endothelial cell injury was determined by MTT and LDH assay. The effect of LTC on lactic dehydrogenase (LDH), nitric oxide (NO), super oxide dlsmutase (SOD) and malondialdehyde (MDA) levels were detected by corresponding assay kits according to manufacturer's instruction. The effect of LTC on the protein expressions of intercellular cell adhesion molecule-1 (ICAM-1), vascular cell adhesion molecule 1 (VCAM-1), p65, p-p65, IKB and p-IKB were detected by Western blot. The results showed that compared with the normal control group, the activity of EAhy.926 cells was significantly decreased, LDH leakage (P<0.01) increased, NO content and SOD activity significantly decreased (P<0.01, P<0.05), and the expressions of ICAM-1, VCAM-1, p-p65/p65 and p-IKB(P<0.05)increased.This study demonstrated that LTC had no significant effect on the growth of normal cells. The treatment with LTC significantly promoted the proliferation of vascular endothelial cells damagedby ox-LDL, decreased MDA content and LDH release, andincreased the activity of SOD and NO content. Meanwhile, ox-LDL significantly increased the expressions of ICAM-1, VCAM-1, p-p65/p65, p-IKB/IKB in Eahy.926 cells; these effects were suppressed by LTC at 1, 2 mg·L⻹. In conclusion, LTC has a significant protective effect on human umbilical vein endothelial cells caused by ox-LDL. This study suggested that LTC has a certain therapeutic effect on AS.
Asunto(s)
Medicamentos Herbarios Chinos/farmacología , Células Endoteliales de la Vena Umbilical Humana/efectos de los fármacos , Lipoproteínas LDL/efectos adversos , Estrés Oxidativo , Células Cultivadas , Humanos , L-Lactato Deshidrogenasa/metabolismo , Malondialdehído/metabolismo , Óxido Nítrico/metabolismo , Superóxido Dismutasa/metabolismoRESUMEN
The "design space" method was used to optimize the purification process of Resina Draconis phenol extracts by using the concept of "quality derived from design" (QbD). The content and transfer rate of laurin B and 7,4'-dihydroxyflavone and yield of extract were selected as the critical quality attributes (CQA). Plackett-Burman design showed that the critical process parameters (CPP) were concentration of alkali, the amount of alkali and the temperature of alkali dissolution. Then the Box-Behnken design was used to establish the mathematical model between CQA and CPP. The variance analysis results showed that the P values of the five models were less than 0.05 and the mismatch values were all greater than 0.05, indicating that the model could well describe the relationship between CQA and CPP. Finally, the control limits of the above 5 indicators (content and transfer rate of laurine B and 7,4'-dihydroxyflavone, as well as the extract yield) were set, and then the probability-based design space was calculated by Monte Carlo simulation and verified. The results of the design space validation showed that the optimized purification method can ensure the stability of the Resina Draconis phenol extracts refining process, which would help to improve the quality uniformity between batches of phenol extracts and provide data support for production automation control.
Asunto(s)
Croton/química , Medicamentos Herbarios Chinos/análisis , Extractos Vegetales/análisis , Resinas de Plantas/análisis , Tecnología Farmacéutica , Modelos Teóricos , Método de Montecarlo , FenolesRESUMEN
To investigate the effect of hot air circulation drying and spray drying on the quality of Tianshu capsule from the view point of chemical compositions. UPLC-DAD was used to establish the fingerprint of Tianshu capsules for the first time, and the main chemical constituents were identified by UPLC-Q-TOF-MS/MS. A total of 62 compounds were identified in this method, 21 of which were reported in Tianshu capsules for the first time. The results showed that there were no significant differences in the identification of the chemical constituents types between these two methods, but the contents of some constituents were different. The common patterns generated by the 10 batches of hot air cycle drying samples were used as the control fingerprint, and the similarity of the spray drying samples fingerprints was 0.877, with high similarity of the fingerprints between these two methods. UPLC-DAD combined with UPLC-Q-TOF-MS/MS technology was used for the first time to evaluate the chemical constituents of Tianshu capsule rapidly, comprehensively and accurately, providing technical support for the quality evaluation of Tianshu capsule.
Asunto(s)
Desecación/métodos , Medicamentos Herbarios Chinos/química , Tecnología Farmacéutica/métodos , Cromatografía Líquida de Alta Presión , Control de Calidad , Espectrometría de Masas en TándemRESUMEN
To establish a UPLC-MS/MS method for simultaneous determination of six triterpenoid constituents (pachymic acid, dehydropachymic acid, dehydrotumulosic acid, polyporenic acid C, dehydroeburicoic acid and dehydrotra metenolic acid) in Guizhi Fuling capsules (GFC). Chromatographic analysis was conducted on Agilent Porosheell 120 SB-C18 column (4.6 mm×150 mm, 2.7 µm), with 0.1% formic acid aqueous solution-methanol as the mobile phase for gradient elution at a flow rate of 0.4 mLâ¢min-1. The column temperature was 30 â and the sample size was 5 µL. The samples were analyzed by tandem mass spectrometer with negative electrospray ionization (ESI) source, and monitored under a multiple reaction monitoring (MRM) mode, with the quantitative ion pairs m/z 527.8â465.5 (pachymic acid), m/z 525.6â465.6 (dehydropachymic acid), m/z 483.4â337.3 (dehydrotumulosic acid), m/z 481.5â419.5 (polyporenic acid C), m/z 467.4â337.1 (dehydroeburicoic acid), m/z 453.4â337.0 (dehydrotra metenolic acid). Six triterpenoid acids showed good linear relationships within the investigated concentration ranges (r> 0.996 8), with RSDs of precision less than 6.2%, and all RSDs of repeatability less than 5.9%. The average recovery rate was 97.90%, 100.2%, 99.60%, 101.7%, 102.6% and 103.0% respectively. The method was rapid, accurate, repeatable and could be used as a method for quantitative determination of triterpenoid acids in Chinese medicine prescriptions, providing a reference method for the quality control of Guizhi Fuling capsules and providing a reference for the content determination for Chinese medicine prescriptions containing Poria cocos.