scholarly journals Characterization and identification of flavonoids from Bambusa chungii leaves extract by UPLC-ESI-Q-TOF-MS/MS

2020 ◽  
Author(s):  
Ting Yuan ◽  
Xue-Feng Guo ◽  
Si-Yue Shao ◽  
Rong-Miao An ◽  
Jin Wang ◽  
...  
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
High Definition ◽  
Bamboo Leaves ◽  
Fat Reduction ◽  
Accurate Mass Measurements ◽  
Acid Aqueous Solution ◽  
Characteristic Fragmentation ◽  
Fragmentation Patterns ◽  
Tof Ms

AbstractBamboo leaves extract (BLE) has a variety of physiological functions such as antitumour, anti-inflammatory, antioxidant and blood fat reduction activities and the flavonoids of bamboo leaves are the major active constituents. To profile the flavonoids in the complex BLE, a rapid and sensitive analytical method based on ultra-high-performance liquid chromatography coupled with electrospray ionization quadrupole time-of-flight tandem mass spectrometry (UPLC-ESI-Q-TOF-MS/MS) was developed for the structural identification of the flavonoids in Bambusa chungii leaves extract using accurate mass measurements and characteristic fragmentation patterns. After separation on an Agilent SB-C18 Rapid Resolution High Definition (RRHD) column (2.1 mm × 150 mm, 1.8 μm) by gradient elution with 0.1% formic acid aqueous solution and acetonitrile as the mobile phase, the sample was analysed by ESI-QTOF-MS/MS in the negative mode. A total of 22 flavonoids were detected, and eight of these were identified by comparison with reference standards, while the other fourteen were tentatively identified according to their MS/MS data. The main fragmentation pathways of flavonoid C-glycosides (compounds 1, 5 and 10), flavonoid di-C,O-glycosides (compound 4), flavonoid di-C-glycosides (compound 7) and flavonoid C,O-di-glycosides (compounds 2 and 14) are shown in this article. This is the first report on the analysis of the flavonoids in the extract of B. chungii leaves. The present work demonstrates that UPLC-ESI-Q-TOF-MS/MS is an efficient technique for identifying multiple flavonoids of BLE.

scholarly journals Chemical Profiles and Simultaneous Quantification of Aurantii fructus by Use of HPLC-Q-TOF-MS Combined with GC-MS and HPLC Methods

Molecules ◽  
2018 ◽  
Vol 23 (9) ◽  
pp. 2189 ◽  
Author(s):  
Yingjie He ◽  
Zongkai Li ◽  
Wei Wang ◽  
Suren Sooranna ◽  
Yiting Shi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
Quality Control ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Gradient Elution ◽  
Chemical Components ◽  
Bioactive Substances ◽  
Flight Mass Spectrometry ◽  
Tof Ms

Aurantii fructus (AF) is a traditional Chinese medicine that has been used to improve gastrointestinal motility disorders for over a thousand years, but there is no exhaustive identification of the basic chemical components and comprehensive quality control of this herb. In this study, high-performance liquid chromatography coupled with quadrupole time of flight mass spectrometry (HPLC-Q-TOF-MS) and gas chromatography coupled mass spectrometry (GC-MS) were employed to identify the basic chemical compounds, and high-performance liquid chromatography (HPLC) was developed to determine the major biochemical markers from AF extract. There were 104 compounds belonging to eight structure types, including 13 amino acids or peptides, seven alkaloids, 18 flavanones, 14 flavones, 15 polymethoxyflavonoids, six triterpenoids, nine coumarins, and 18 volatile oils, as well as four other compounds that were systematically identified as the basic components from AF, and among them, 41 compounds were reported for the first time. Twelve bioactive ingredients were chosen as the benchmark markers to evaluate the quality of AF. The analysis was completed with a gradient elution at a flow rate of 0.7 mL/min within 55 min. This efficient method was validated showing good linearity, precision, stability, repeatability and recovery. Furthermore, the method was successfully applied to the simultaneous determination of 12 chemical markers in different samples of AF. This study could be applied to the identification of multiple bioactive substances and improve the quality control of AF.

Some Aspects of the Mass Spectra of.N-Nitrosamines

1971 ◽  
Vol 49 (9) ◽  
pp. 1367-1371 ◽  
Author(s):  
J. W. ApSimon ◽  
J. D. Cooney
Keyword(s):  
Mass Spectra ◽  
Accurate Mass ◽  
Mass Measurements ◽  
Molecular Ion ◽  
Accurate Mass Measurements ◽  
Characteristic Fragmentation ◽  
Fragmentation Patterns

The mass spectra of seven cyclic N-nitrosamines were examined for characteristic fragmentation patterns. Accurate mass measurements on three of the compounds indicated that the M-17 and M-30 peaks resulted from molecular ion losses of •OH and •NO respectively. The loss of • OH was rationalized in terms of a McLafferty-type rearrangement.

scholarly journals Metabolite Profiling of Meridianin C In Vivo of Rat by UHPLC/Q-TOF MS

2021 ◽  
Vol 2021 ◽  
pp. 1-10
Author(s):  
Guozhe Zhang ◽  
Linxia Xiao ◽  
Liang Qi
Keyword(s):  
High Performance ◽  
Kinase Inhibitor ◽  
Solid Phase ◽  
Extraction Methods ◽  
Mass Spectral Fragmentation ◽  
Mass Spectral ◽  
Flight Mass Spectrometry ◽  
Fragmentation Patterns ◽  
Tof Ms

Meridianin C (MC), as a marine alkaloid, is a potent protein kinase inhibitor which exhibits good anticancer activity. However, the in vivo metabolism of MC has not been described to date. In this study, an ultra-high performance liquid chromatography/quadrupole time-of-flight mass spectrometry (UHPLC/Q-TOF MS) method is employed to investigate the in vivo metabolites of MC in rats. Plasma, bile, urine, and feces are collected after a single oral dose of MC. Protein precipitation, solid phase extraction (SPE), and ultrasonic extraction methods are used to prepare samples. Based on the mass spectral fragmentation patterns, elution order, and retrieving literatures, a total of 13 metabolites of MC were detected and tentatively identified, utilizing MetaboLynx software. The metabolic pathways of MC in rats include N- or O-glucuronidation, O-sulfation, N-hydroxylation, dihydroxylation, and trihydroxylation. The relative content of the metabolites in each kinds of biological samples is also evaluated. This study will help to understand the in vivo properties of MC for the future usage.

scholarly journals HPLC–MS/MS profiling of wild-growing scentless chamomile

2020 ◽  
Vol 32 (2) ◽  
pp. 86-94 ◽  
Author(s):  
Filip Šibul ◽  
Dejan Orčić ◽  
Sanja Berežni ◽  
Goran Anačkov ◽  
Neda Mimica-Dukić
Keyword(s):  
High Performance ◽  
Quinic Acid ◽  
Human Consumption ◽  
Plant Metabolites ◽  
Liquid Chromatography Tandem Mass ◽  
Health Promoting ◽  
Tandem Mass Spectroscopy ◽  
The Common ◽  
Characteristic Fragmentation ◽  
Fragmentation Patterns

Scentless chamomile (Tripleurospermum inodorum = M. inodora) is a plant belonging to Anthemideae tribe of Asteraceae family, with phenotype similar to the common chamomile, a plant used in human consumption in the form of herbal tea infusion. In order to be able to understand possible health-promoting properties and adverse effects of the scentless chamomile's consumption, it is of essence to examine its chemical composition. The aim of the study was to perform phenolic profiling using high-performance liquid chromatography–tandem mass spectroscopy (HPLC–MS/MS), in comparison to the common chamomile. In the investigated extracts, qualitative and quantitative analyses enabled the identification of 66 compounds based on their retention times, mass (MS/MS) spectra, and analysis of their characteristic fragmentation patterns in MS/MS Product Ion Scan experiments. A new HPLC–MS/MS method for quantitation of common plant metabolites was hereby developed, enabling quantitation of 47 compounds. All examined M. inodora samples have relatively high combined phenolic and flavonoid contents (25.2–51.9 mg/g). Apigenin, apigenin-7-O-glucoside, luteolin, luteolin-7-O-glucoside, quinic acid, and 5-O-caffeoyl quinic acid were the compounds with highest concentration in both inodorous and common chamomile. The results obtained hereby represent the first and most detailed chemical profile of scentless chamomile so far.

scholarly journals Quantitative Determination of 7 Saikosaponins in Xiaochaihu Granules Using High-Performance Liquid Chromatography with Charged Aerosol Detection

2021 ◽  
Vol 2021 ◽  
pp. 1-7
Author(s):  
Aoxue Liu ◽  
Tongtong Xu ◽  
Wenning Yang ◽  
Dandan Zhou ◽  
Yiwei Sha
Keyword(s):  
High Performance ◽  
Gradient Elution ◽  
Charged Aerosol Detection ◽  
Charged Aerosol ◽  
Relative Standard ◽  
Acid Aqueous Solution ◽  
Bupleuri Radix ◽  
Interday Precision

Bupleuri Radix (Chaihu, in Chinese) is the principal drug in Xiaochaihu granules (XGs) that is a famous Chinese medicine preparation in China. Since previous analytical methods have not focused on the multiactive saikosaponins of Chaihu, it is difficult to effectively control the quality of XG on the market. In this manuscript, the simultaneous determination of 7 saikosaponins (saikosaponins C, I, H, A, B2, G, and B1) in XG by HPLC with charged aerosol detection (CAD) and confirmation by LC-Q-Orbitrap HRMS were described. The saikosaponins were purified on an SPE cartridge and determined on a Waters CORTECTS C18 column (4.6 mm × 150 mm, 2.7 μm) by gradient elution using 0.01% acetic acid aqueous solution and acetonitrile. The results showed good linearity with the r2 values higher than 0.998 for all analytes. The average recoveries at three different concentration levels ranged from 80% to 109% and the intraday and interday precision (relative standard deviations, RSD%) were in the range of 1.0%∼1.9% and 1.4%∼2.1%, respectively. The established HPLC-CAD method was subsequently applied to 15 batches of XG to investigate the batch-to-batch consistency and controllability. The proposed method could potentially be used for the quality control of XG and also be helpful in the quality evaluation of Chaihu and its related preparations.

Reversed-Phase High Performance Liquid Chromatographic Analysis of Three First Line Anti-Tuberculosis Drugs

2019 ◽  
Vol 69 (12) ◽  
pp. 3590-3592
Author(s):  
Nela Bibire ◽  
Romeo Iulian Olariu ◽  
Luminita Agoroaei ◽  
Madalina Vieriu ◽  
Alina Diana Panainte ◽  
...  
Keyword(s):  
High Performance ◽  
Biological Fluids ◽  
Gradient Elution ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Assay Method ◽  
Active Pharmaceutical Ingredients ◽  
First Line ◽  
Pharmaceutical Ingredients ◽  
Liquid Chromatographic

Active pharmaceutical ingredients such as isoniazid, pyrazinamide and rifampicin are among the most important first-line anti-tuberculosis drugs. A simple, rapid and sensitive reversed phase-high performance liquid chromatographic assay method for the simultaneous determination of isoniazid, pyrazinamide and rifampicin has been developed. Separation of the interest compounds was achieved in a 10 min chromatographic run in gradient elution mode on a Zorbax SB-C18 stainless steel column (150 � 4 mm, 5 mm) using a guard column containing the same stationary phase. The gradient elution was carried out with a mobile phase of 10% CH3CN aqueous solution for channel A and 50% CH3CN in pH = 6.8 phosphate buffer (20 mM), to which 1.5 mL triethylamine were added for channel B. Quantification of the analyzed substances was carried out spectrophotometrically at 269 nm. Detection limits of 0.48 mg/L for isoniazid, 0.52 mg/L for pyrazinamide and 0.48 mg/L for rifampicin were established for the developed assay method. The present work showed that the proposed analysis method was advantageous for simple and rapid analysis of the active pharmaceutical ingredients in pharmaceuticals and biological fluids.

Simultaneous Determination of Eight Potential Q-Markers in Zishen Tongguan Capsules Based on UHPLC-MS/MS

2020 ◽  
Vol 17 (1) ◽  
pp. 47-56
Author(s):  
Shun Liu ◽  
Xun Wang ◽  
Kaiping Zou ◽  
Wei Liu ◽  
Cunyu Li ◽  
...  
Keyword(s):  
Quality Control ◽  
Chinese Medicine ◽  
Simultaneous Determination ◽  
High Performance ◽  
Multiple Reaction Monitoring ◽  
Gradient Elution ◽  
Quality Markers ◽  
High Repeatability ◽  
Comprehensive Study

Background: Zishen Tongguan (ZSTG) capsules were prepared at the Affiliated Hospital of Nanjing University of Chinese Medicine and have been proven to be clinically effective for treating pyelonephritis and benign prostatic hyperplasia. However, the quality standards are not ideal; a comprehensive study of the “quality markers” (Q-markers), the chemicals inherent in traditional Chinese medicine and its preparations, has not been carried out. Experimental Methods: In this paper, a sensitive and specific ultra-high-performance liquid chromatographictandem mass spectrometry (UHPLC-MS/MS) method was developed for the simultaneous determination of eight potential Q-markers of ZSTG, including timosaponin A3, berberine, jatrorrhizine, phellodendrine, palmatine, mangiferin, neomangiferin, and timosaponin BII. A Kromasil 100-3.5 C18 column was used with a mobile phase of 0.2% formic acid with acetonitrile, and gradient elution at a flow rate of 0.2 mL/min was achieved in 13 minutes and used for separation. Detection was performed in positive/negative mode with multiple reaction monitoring (MRM). Results: The analytical method was validated in terms of the sensitivity, linearity, accuracy, precision, repeatability, stability and recovery. The method established here was successfully applied to study the potential Q-markers in 8 batches of commercial samples, which demonstrated its use in improving the quality control of ZSTG. Conclusion: The developed method had high repeatability and accuracy and was suitable for the simultaneous analysis of multiple Q-markers, which may provide a new basis for the comprehensive assessment and overall quality control of ZSTG.

Analysis of organic impurities of besifloxacin hydrochloride by high performance liquid chromatography with isocratic and gradient elution.

2019 ◽  
Vol 16 ◽  
Author(s):  
Joanna Wittckind Manoel ◽  
Camila Ferrazza Alves Giordani ◽  
Livia Maronesi Bueno ◽  
Sarah Chagas Campanharo ◽  
Elfrides Eva Sherman Schapoval ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Mobile Phase ◽  
High Performance ◽  
Gradient Elution ◽  
Pharmaceutical Product ◽  
Raw Material ◽  
Isocratic Elution ◽  
Organic Impurities ◽  
Elution Method

Introduction: Impurity analysis is an important step in the quality control of pharmaceutical ingredients and final product. Impurities can arise from drug synthesis or excipients and even at small concentrations may affect product efficacy and safety. In this work two methods using high performance liquid chromatography (HPLC) were developed and validated for the evaluation of besifloxacin and its impurity synthesis, with isocratic elution and another with gradient elution. Method: The analysis by HPLC in isocratic elution mode was performed using a cyano column maintained at 25 °C. The mobile phase was composed by 0.5% triethylamine (pH 3.0): acetonitrile (88:12 v/v) eluted at a flow rate of 1.0 ml/min with detection at 330 nm. The gradient elution method was carried out with the same column and mobile phase components only modifying the rate between organic and aqueous phase during analysis. The procedures have been validated according to internationally accepted guidelines, observing results within acceptable limits. Results: The methods presented were found to be linear in the 140 to 260 µg/ml range for besifloxacin and 0.3 to 2.3 µg/ml for an impurity named A. The limits of detection and quantification were respectively 0.07 and 0.3 µg/ml for impurity A, with a 20 µL injection volume. The precision achieved for all analyses performed provided RSD inter-day equal to 6.47 and 6.36% for impurity A with isocratic elution and gradient, respectively. The accuracy was higher than 99% and robustness exhibited satisfactory results. In the isocratic method an analysis time of 25 min and 15 min was obtained for gradient. For impurity A, the number of theoretical plates in the isocratic mode was about 5000 while in the gradient mode it was about 45000, hence, it made the column more efficient by changing the mobile phase composition during elution. In besifloxacin raw material and in pharmaceutical product used in this study, other related impurities were present but but impurity A was searched for and not detected Conclusion: The proposed methods can be applied for quantitative determination of impurities in the analysis of the besifloxacin raw material, as well as in ophthalmic suspension of the drug, considering the quantitation limit.

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