scholarly journals Rapid Identification of the Multiple Absorbed Bioactive Components and Metabolites in Rat Serum after Oral Administration of Wu-Jia Sheng-Hua Capsule by UPLC-ESI-MS

2013 ◽  
Vol 2013 ◽  
pp. 1-6 ◽  
Author(s):  
Fang Geng ◽  
Fashan Wang ◽  
Taobo Zou ◽  
Kuiyuan Zhu ◽  
Wei Ma ◽  
...  

To identify the compounds absorbed in rat serum after the oral administration of Wu-Jia Sheng-Hua (WJSH) capsule, a traditional Chinese medicine (TCM) compound prescription, an ultraperformance liquid chromatography coupled with electrospray ionization mass spectrometry (UPLC/ESI-MS) method, was established. The chromatographic separation of the absorbed compounds and metabolites was achieved with an ACQUITY UPLC BEH C18 column (2.1 mm×50 mm, 1.7 μm) under a gradient elution. The mobile phase was composed of acetonitrile and water buffered with ammonium acetate (10 mM) and formic acid (0.1%, V/V). Twelve absorbed compounds and four metabolites were found. Seven of the absorbed compounds were identified by ESI-MS. The identification of absorbed compounds might be helpful for the better understanding of the mechanisms underlying the pharmacological effects of WJSH capsule.

Author(s):  
Jinglong Wang ◽  
Dandan Zheng ◽  
Nan Xu ◽  
Chao Zhang ◽  
Yingzi Wang ◽  
...  

AbstractTo realize the attribution and identification of absorbed components in rat serum after oral administration of Erhuang decoction prepared by semi-bionic enzyme extraction method, the fingerprints of serum samples were established using a HPLC-DAD-ESI-MS method. Thirty-two peaks in Erhuang decoction and 24 peaks in rat serum after oral administration of Erhuang decoction were detected. Among the 24 peaks detected in rat serum, 25 compounds were identified by comparing the retention time and mass spectrometry data with that of reference compounds, or by mass spectrometry analysis and retrieving the reference literatures. Among the identified 25 compounds in vivo, 24 were the original form of compounds absorbed from the detected compounds in vitro, and one was the metabolite compounds of licorice. By analyzing the mass spectrometry or ultraviolet absorption characteristics, other unidentified compounds in vivo were deduced to be the endogenous metabolites in serum or the original form and metabolites of the compounds existed in vivo. Results indicated that HPLC-DAD-ESI-MS is suitable for identifying the bioactive constituents in serum after oral administration of Erhuang decoction, and the findings would be beneficial to further research and development of the pharmacodynamic substance base of Erhuang decoction.


2020 ◽  
Vol 19 (3) ◽  
pp. 651-659
Author(s):  
Xin Jia ◽  
Yinfei Du ◽  
Jia Xu ◽  
Yu Dong

Purpose: To develop a simple, rapid and sensitive ultra-performance liquid chromatography - electrospray ionization-mass spectrometry (UPLC–ESI–MS/MS) method was developed and fully validated for the simultaneous determination of galangin, kaempferide, galangin-3-methylether, kaempferol and quercetin in rat plasma after oral administration of Mongolian Medicine, Shudage-4 extracts. Methods: The galangin, kaempferide, galangin-3-methylether, kaempferol and quercetin were separated on a C18 column using 0.1 % formic acid at a flow rate of 0.4 mL / min and detected by a mass spectrometer in negative-ion mode with selected reaction monitoring (SRM) mode. Plasma samples were processed with a simple deproteinization technique using ethyl acetate and acetonitrile. Following the protein precipitation, the plasma samples were evaporated under gentle stream of nitrogen and analyzed by above method. Naringin was used as an internal standard (IS). Method validation was performed according to the Chinese Food and Drug Administration guidelines. Results: A good linearity (r2 ≥ 0.9990) was showed by the UPLC – ESI – MS / MS method, the low limits of quantification for galangin, kaempferide, galangin-3-methylether, kaempferol and quercetin were 229.8, 78.8, 32.0, 123.7 and 137.8 ng / mL, respectively. The results of inter-day and intra-day precisions met the experimental requirement (< 7.8 %). The matrix effect and recovery efficiency of the five analytes were more than 72.9 and 88.7 % respectively. The stability of the analytes were satisfactory. The UPLC – ESI – MS / MS method has been used for the five analytes’ pharmacokinetics study successfully after gastrointestinal route of the Mongolian Medicine Shudage-4. The pharmacokinetic parameters showed significant differences (P < 0.05) between the normal and gastric ulcer groups. The metabolism and transport of the five analytes in gastric ulcer rates were faster than in normal rats after administration of Shudage - 4 extract. Double-peak phenomenon appeared in galangin, galangin – 3 - methylether and quercetin. Conclusion: The results suggest that the metabolism and transport of Mongolian Medicine Shudage-4 in gastric ulcer rats is faster than in normal rats and may be enriched and acted on at the lesion site. Keywords: UPLC – ESI – MS / MS; Mongolian medicine; Shudage - 4; pharmacokinetics; gastric ulcer


2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Yulu Zhou ◽  
Ting Zhou ◽  
Qi Pei ◽  
Shikun Liu ◽  
Hong Yuan

Chlorogenic acid (ChA) is proposed as the major bioactive compounds of Lonicerae Japonicae Flos (LJF). Forty-two Wistar rats were randomly divided into seven groups to investigate the pharmacokinetics and tissue distribution of ChA, via oral administration of LJF extract, using ibuprofen as internal standard, employing a high performance liquid chromatography in conjunction with tandem mass spectrometry. Analytes were extracted from plasma samples and tissue homogenate by liquid–liquid extraction with acetonitrile, separated on a C18 column by linear gradient elution, and detected by electrospray ionization mass spectrometry in negative selected multiple reaction monitoring mode. Our results successfully demonstrate that the method has satisfactory selectivity, linearity, extraction recovery, matrix effect, precision, accuracy, and stability. Using noncompartment model to study pharmacokinetics, profile revealed that ChA was rapidly absorbed and eliminated. Tissue study indicated that the highest level was observed in liver, followed by kidney, lung, heart, and spleen. In conclusion, this method was suitable for the study on pharmacokinetics and tissue distribution of ChA after oral administration.


Molecules ◽  
2021 ◽  
Vol 26 (8) ◽  
pp. 2284
Author(s):  
Fernanda das Neves Costa ◽  
Gerold Jerz ◽  
Peter Hewitson ◽  
Fabiana de Souza Figueiredo ◽  
Svetlana Ignatova

The detailed metabolite profiling of Laguncularia racemosa was accomplished by high-performance countercurrent chromatography (HPCCC) using the three-phase system n-hexane–tert-butyl methyl ether–acetonitrile–water 2:3:3:2 (v/v/v/v) in step-gradient elution mode. The gradient elution was adjusted to the chemical complexity of the L. racemosa ethyl acetate partition and strongly improved the polarity range of chromatography. The three-phase solvent system was chosen for the gradient to avoid equilibrium problems when changing mobile phase compositions encountered between the gradient steps. The tentative recognition of metabolites including the identification of novel ones was possible due to the off-line injection of fractions to electrospray ionization mass spectrometry (ESI-MS/MS) in the sequence of recovery. The off-line hyphenation profiling experiment of HPCCC and ESI-MS projected the preparative elution by selected single ion traces in the negative ionization mode. Co-elution effects were monitored and MS/MS fragmentation data of more than 100 substances were used for structural characterization and identification. The metabolite profile in the L. racemosa extract comprised flavonoids, hydrolysable tannins, condensed tannins and low molecular weight polyphenols.


2019 ◽  
Vol 15 (5) ◽  
pp. 505-510
Author(s):  
Yanjuan Zheng ◽  
Qiushi Peng ◽  
Rui Dong ◽  
Tingyu Chen ◽  
Yi Bao ◽  
...  

Introduction: A rapid, and accurate Ultra Performance Liquid Chromatography (UPLC) method was developed to simultaneously analyze Methocarbamol, Paracetamol and the related substances Materials and Methods: Waters ACQUITY UPLC® BEH Phenyl C18 column was used in conjunction with UV detection at 225nm. Gradient elution with 0.05M, pH 6 phosphate buffer and acetonitrile flow at 0.3mL /min rate were used to separate the substances. The retention times for 4-Aminopheno, Paracetamol, Guaifenesin, Methocarbamol, and 4-Chloroacetanilide were 1.319 minute, 2.224 minute, 4.467 minute, 4.769 minute and 5.433 minute respectively. The concentration was linear in the range of 2-100 µg/ml for Methocarbamol, and 1-100 µg/mL for Paracetamol. The percentage recoveries were between 99.28±1.23% to 100.57±0.99% for Methocarbamol, and between 99.08±1.23% to 101.23±1.39% for Paracetamol. Results and Discussion: The validated optimal protocol is robust and accurate for simultaneous analysis of Methocarbamol, Paracetamol and the related substances, applicable for bulk powder as well as pharmaceutical formulation. Conclusion: In this paper, a highly sensitive, accurate, and precise UPLC method with UV-Vis detection was developed and validated for quality control of MET and PAR in bulk as well as in pharmaceutical preparations.


2019 ◽  
Vol 15 (2) ◽  
pp. 121-129
Author(s):  
Zhi Rao ◽  
Bo-xia Li ◽  
Yong-Wen Jin ◽  
Wen-Kou ◽  
Yan-rong Ma ◽  
...  

Background: Imatinib (IM) is a chemotherapy medication metabolized by CYP3A4 to Ndesmethyl imatinib (NDI), which shows similar pharmacologic activity to the parent drug. Although methods for determination of IM and/or NDI have been developed extensively, only few observations have been addressed to simultaneously determine IM and NDI in biological tissues such as liver, kidney, heart, brain and bone marrow. Methods: A validated LC-MS/MS method was developed for the quantitative determination of imatinib (IM) and N-desmethyl imatinib (NDI) from rat plasma, bone marrow, brain, heart, liver and kidney. The plasma samples were prepared by protein precipitation, and then the separation of the analytes was achieved using an Agilent Zorbax Eclipse Plus C18 column (4.6 × 100 mm, 3.5 µm) with gradient elution running water (A) and methanol (B). Mass spectrometric detection was achieved by a triplequadrupole mass spectrometer equipped with an electrospray source interface in positive ionization mode. Results: This method was used to investigate the pharmacokinetics and the tissue distributions in rats following oral administration of 25 mg/kg of IM. The pharmacokinetic profiles suggested that IM and NDI are disappeared faster in rats than human, and the tissue distribution results showed that IM and NDI had good tissue penetration and distribution, except for the brain. This is the first report about the large penetrations of IM and NDI in rat bone marrow. Conclusion: The method demonstrated good sensitivity, accuracy, precision and recovery in assays of IM and NDI in rats. The described assay was successfully applied for the evaluation of pharmacokinetics and distribution in the brain, heart, liver, kidney and bone marrow of IM and NDI after a single oral administration of IM to rats.


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