Profiling and Quantification of the Key Phytochemicals from the Drumstick Tree (Moringa oleifera) and Dietary Supplements by UHPLC-PDA-MS

Planta Medica ◽  
2020 ◽  
Author(s):  
Omer I. Fantoukh ◽  
Yan-Hong Wang ◽  
Abidah Parveen ◽  
Mohammed F. Hawwal ◽  
Gadah A. Al-Hamoud ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Dietary Supplements ◽  
High Performance ◽  
Moringa Oleifera ◽  
Negative Ion ◽  
Array Detector ◽  
Ionization Mass ◽  
Fractionation Process ◽  
Chromatography Method ◽  
Drumstick Tree

Abstract Moringa oleifera is known as a drumstick tree and is cultivated in the subtropics and tropics. It exhibits antihypertensive and antidiabetic effects. An ultra-high-performance liquid chromatography method was developed for the determination of 9 phytochemicals in M. oleifera leaves and marketed products. The efficient separation was achieved within 7 min with a temperature of 45 °C by using a C-18 column as the stationary phase and water/acetonitrile with 0.05% formic acid as the mobile phase. The method was validated for linearity, repeatability, limits of detection, and limits of quantification. The limits of detections of phenolic compounds 1 – 9 were as low as 0.2 µg/mL. The photodiode array detector at 220 and 255 nm wavelengths was recruited for quantification. The key phytochemicals were detected in the range of 0.42 to 2.57 mg/100 mg sample weight in 13 dietary supplements. This study considers the quantitative analysis for lignans in M. oleifera for the first time. Isoquercitrin (5) and quercetin 3-O-(6-O-malonyl)-β−D-glucopyranoside (6) predominates the leaves of M. oleifera with inherent degradable nature detected for compound 6. Niazirin (2) was detected in amounts between 0.010 – 0.049 mg/100 mg while compound 1 was undetectable and potentially an artifact because of the fractionation process. The characterization and confirmation of components were achieved by liquid chromatography-electrospray ionization-mass spectrometry with extractive ion monitoring for the positive and negative ion modes. The developed and validated method is robust and rapid in the conclusive quantification of phytochemicals and authentication of the Moringa samples for quality assurance.

Quantification of Phenolic Compounds from Fadogia agrestis and Dietary Supplements using UHPLC-PDA-MS

Planta Medica ◽  
2018 ◽  
Vol 85 (02) ◽  
pp. 145-153 ◽  
Author(s):  
Bharathi Avula ◽  
Ji-Yeong Bae ◽  
Vijayasankar Raman ◽  
Omer Fantoukh ◽  
Yan-Hong Wang ◽  
...  
Keyword(s):  
Liquid Chromatography ◽  
Phenolic Compounds ◽  
Dietary Supplements ◽  
High Performance ◽  
Chemical Constituents ◽  
Array Detector ◽  
Gradient System ◽  
Chromatography Method ◽  
Limits Of Detection ◽  
Positive Mode

Abstract Fadogia agrestis is used in traditional African medicine as an analgesic and for anti-inflammatory and aphrodisiac activities. An ultra-high-performance liquid chromatography method was developed for the determination of 11 chemical constituents from roots and aerial parts of F. agrestis. The separation was achieved within 7 min by using C-18 column material and a water/acetonitrile mobile phase, both containing 0.1% formic acid gradient system with a temperature of 45 °C. The method was validated for linearity, repeatability, limits of detection, and limits of quantification. The limits of detection of phenolic compounds were found to be in the range from 0.025 to 0.1 µg/mL. The wavelengths used for quantification with the photodiode array detector were 238, 254, 291, and 325 nm. Twelve of 17 dietary supplements contained phenolic compounds in the range from 0.3 to 2.7 mg/d. The phenolic compounds were not detected in five dietary supplements. Liquid chromatography-mass spectrometry coupled with electrospray ionization interface method is described for the identification and confirmation of compounds from plant samples and dietary supplements claiming to contain F. agrestis. This method involved the use of [M + H]+ and [M + Na]+ ions in the positive mode and [M − H]− ions in the negative mode with extractive ion monitoring. The developed method is simple, economic, rapid, and especially suitable for quality control and chemical fingerprint analysis of F. agrestis.

scholarly journals Simultaneous Extraction Optimization and Analysis of Flavonoids from the Flowers of Tabernaemontana heyneana by High Performance Liquid Chromatography Coupled to Diode Array Detector and Electron Spray Ionization/Mass Spectrometry

2013 ◽  
Vol 2013 ◽  
pp. 1-10 ◽  
Author(s):  
Thiyagarajan Sathishkumar ◽  
Ramakrishnan Baskar ◽  
Mohan Aravind ◽  
Suryanarayanan Tilak ◽  
Sri Deepthi ◽  
...  
Keyword(s):  
Mass Spectrometry ◽  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Shake Flask ◽  
Orthogonal Design ◽  
Array Detector ◽  
Diode Array ◽  
Ionization Mass ◽  
Diode Array Detector

Flavonoids are exploited as antioxidants, antimicrobial, antithrombogenic, antiviral, and antihypercholesterolemic agents. Normally, conventional extraction techniques like soxhlet or shake flask methods provide low yield of flavonoids with structural loss, and thereby, these techniques may be considered as inefficient. In this regard, an attempt was made to optimize the flavonoid extraction using orthogonal design of experiment and subsequent structural elucidation by high-performance liquid chromatography-diode array detector-electron spray ionization/mass spectrometry (HPLC-DAD-ESI/MS) techniques. The shake flask method of flavonoid extraction was observed to provide a yield of 1.2±0.13 (mg/g tissue). With the two different solvents, namely, ethanol and ethyl acetate, tried for the extraction optimization of flavonoid, ethanol (80.1 mg/g tissue) has been proved better than ethyl acetate (20.5 mg/g tissue). The optimal conditions of the extraction of flavonoid were found to be 85°C, 3 hours with a material ratio of 1 : 20, 75% ethanol, and 1 cycle of extraction. About seven different phenolics like robinin, quercetin, rutin, sinapoyl-hexoside, dicaffeic acid, and two unknown compounds were identified for the first time in the flowers of T. heyneana. The study has also concluded that L16 orthogonal design of experiment is an effective method for the extraction of flavonoid than the shake flask method.

scholarly journals Recognition and Optimization of Ingredients Treating Nitroglycerin-Induced Migraine Rats from Wuzhuyu Decoction

2019 ◽  
Vol 2019 ◽  
pp. 1-15 ◽  
Author(s):  
Yongsong Xu ◽  
Sha Wu ◽  
Yanchuan Wu ◽  
Muxin Gong ◽  
Zhimin Wang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Correlation Analysis ◽  
Absorption Spectra ◽  
High Performance ◽  
Uniform Design ◽  
Array Detector ◽  
Least Squares Regression ◽  
Chromatography Method ◽  
Entropy Weighted

Wuzhuyu decoction (WZYD) has been clinically used to treat migraine effectively since Eastern Han Dynasty of ancient China. However, its antimigrainic ingredients remain unclear. In present study, the antimigrainic ingredients of WZYD were explored and optimized in nitroglycerin-induced migraine rats through correlation analysis of decoction spectra-pharmacological effects and absorption spectra-pharmacological using entropy-weighted partial least squares regression method. The decoction spectra and absorption spectra were obtained through the determination of nine main ingredients in ten kinds of WZYDs and WZYDs’ single-pass intestinal perfusion samples using high performance liquid chromatography-diode array detector. The pharmacodynamics indexes related to migraine model rats were detected using high performance liquid chromatography method and kits after oral administration of WZYDs. Then, the key ingredients influencing indexes were achieved through the correlation analysis. And the optimization of key ingredients was acquired through uniform design experiment. The pharmacodynamic verification test was used to clarify the advantages of the optimized sample. The results showed that the final optimized sample, in which the concentrations of rutaecarpine, evodiamine, ginsendside Rb1, 6-gingerol, ginsendside Rg1, rutaevine, and limonin were 0.081, 0.565, 1.455, 0.159, 0.871, 0.178, and 0.009 mg·mL−1, respectively, provided the best comprehensive effect than another optimized sample and the best uniform design sample. Therefore, a new reliable method for rapidly recognizing and optimizing the effective constituents of WZYD treating migraine was established.

scholarly journals DEVELOPMENT OF A HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD FOR ANALYZING DISODIUM 5′-GUANYLATE AND DISODIUM 5′-INOSINATE LEVELS IN FLAVOR ENHANCERS

2018 ◽  
Vol 10 (1) ◽  
pp. 133
Author(s):  
Dwi Karina Natalia ◽  
Harmita . ◽  
Taufiq Indra Rukmana
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
High Performance ◽  
Potassium Phosphate ◽  
Array Detector ◽  
Potassium Phosphate Buffer ◽  
Chromatography Method

Objective: This study aimed to develop a selective analytical method for assessing disodium 5′-guanylate and disodium 5′-inosinate levels in flavorenhancers.Methods: The levels were assessed using high-performance liquid chromatography (HPLC) with a photodiode array detector (PDA) (wavelength=255 nm) and a SunFire® C18 column (250 mm × 4.6 mm × 5 μm). The mobile phase comprised a mixture of potassium phosphate buffer and anion pair reagent-hexane-1-sulfonic acid sodium salt - with a flow rate of 1.2 mL/min. The ion pair was used to generate a neutral equilibrium, whichresulted in increased retention of the analytes. Optimized analysis conditions were then validated regarding accuracy, precision, linearity, selectivity,and the limits of detection and quantification.Results: The average levels of disodium 5′-inosinate in the six analyzed samples were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and0.47±2.21%, respectively. Regarding disodium 5′-guanylate, the average levels were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and0.34±1.83, respectively.Conclusion: The optimal conditions for analyzing disodium 5′-guanylate and disodium 5′-inosinateusing HPLC with a PDA and SunFire C18 columnwere λ=255 nm, a mobile phase of potassium phosphate buffer and sodium hexane sulfonate, and a flow rate of 1.2 mL/min. For disodium 5′-inosinate,its average levels in samples A–F were 0.24±1.46, 0.21±2.69, 0.58±3.26, 0.21±0.84, 0.22±3.59, and 0.47±2.21%, respectively. Meanwhile, the averagelevels of disodium 5′-guanylate in the samples were 0.15±2.85, 0.15±0.12, 0.41±3.80, 0.16±1.72, 0.27±1.18, and 0.34±1.83%, respectively.

Simultaneous determination of ciprofloxacin hydrochloride and hydrocortisone in ear drops by high performance liquid chromatography

2014 ◽  
Vol 68 (7) ◽  
Author(s):  
Joanna Ronowicz ◽  
Bogumiła Kupcewicz ◽  
Łukasz Pałkowski ◽  
Piotr Bilski ◽  
Tomasz Siódmiak ◽  
...  
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Limit Of Detection ◽  
Array Detector ◽  
Chromatography Method ◽  
Ciprofloxacin Hydrochloride ◽  
Validation Parameters ◽  
Limit Of Quantitation ◽  
Ear Drops

AbstractThe aim of the study was to design and validate a reversed phase high performance liquid chromatography method for the separation and quantification of two active pharmaceutical ingredients (ciprofloxacin hydrochloride, hydrocortisone) and a preservative (benzyl alcohol) in ear drops. Effective separation of the examined compounds was achieved on a GraceSmart™ RP 18 column (150 mm × 4.6 mm, 5 μm) with gradient elution and a diode array detector. The total assay run time was 25 min. Analytical method validation assays were performed. Validation parameters used for the evaluation were: specificity, linearity, trueness, precision (repeatability and reproducibility), limit of detection and limit of quantitation. Results of the validation procedure (high recoveries, good standard deviations, no interfering peaks at the retention times corresponding to the analytes) confirm that the developed chromatographic method can be applied for routine analysis of ear drops.

scholarly journals A comparative study of HPLC-DAD and UPLC-UV methods for simultaneous determination of 11 polyphenols in Moringa oleifera leaves

2021 ◽  
Vol 20 (11) ◽  
pp. 2371-2379
Author(s):  
Yanqin Zhu ◽  
Qinhong Yin ◽  
Yaling Yang
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
High Performance ◽  
Moringa Oleifera ◽  
Accurate Determination ◽  
Gradient Elution ◽  
Hplc Method ◽  
Array Detector ◽  
Moringa Oleifera Leaves

Purpose: To develop, validate and compare two chromatographic methods - high performance liquid chromatography with diode array detector ((HPLC-DAD) and high performance liquid chromatography with ultraviolet detection (UPLC-UV) for the effective analysis of polyphenols in Moringa oleifera leaves.Methods: HPLC-DAD and UPLC-UV methods were applied for the accurate determination of eleven major polyphenols in Moringa oleifera leaves. The chromatographic conditions of the eleven polyphenols was determined on two C18 column by gradient elution with 0.5 % phosphoric acid solution -acetonitrile as the eluate, and at a flow rate of 1.0 and 0.5 mL/min for HPLC-DAD and UPLC-UV methods, respectively. Detector parameter of UPLC-UV was fixed at 203 nm. The assay methods were validated systematically.Results: The instrumental methods (HPLC-DAD and UPLC-UV) had good linearity, precision,repeatability and recovery. For both methods, quantification limits of UPLC-UV (0.057 - 0.363 μg/mL) were lower than those of UPLC-UV (0.094 - 1.532 μg/mL). The UPLC method with a shorter running time and more sensitive detection was applied in comparing to the HPLC method. After optimization and evaluation, the baseline of 11 compounds was separated effectively within 68 and 34 min, respectively.Conclusion: The developed HPLC-DAD and UPLC-UV assays were successfully utilized for thesimultaneous analysis of eleven major polyphenols and can readily be utilized as quality control tools for Moringa oleifera leaves in China, with UPLC-UV method showing better separation, lower organic solvent usage and shorter analytical period.

scholarly journals QUALITY BY DESIGN APPROACH TO STABILITY-INDICATING REVERSE-PHASE HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY METHOD DEVELOPMENT, OPTIMIZATION, AND VALIDATION FOR THE ESTIMATION OF SIMEPREVIR IN BULK DRUG

2019 ◽  
pp. 93-100
Author(s):  
VANITHA C ◽  
SATYANARAYANA SV ◽  
BHASKAR REDDY K
Keyword(s):  
Liquid Chromatography ◽  
Flow Rate ◽  
High Performance ◽  
Method Development ◽  
Quality By Design ◽  
Polynomial Equation ◽  
Array Detector ◽  
Reverse Phase ◽  
Chromatography Method ◽  
Stability Indicating

Objective: A simple, robust, precise, and selective stability-indicating liquid chromatography (LC) method (reverse-phase high-performance LC) was developed for the estimation of simeprevir through quality by design paradigm. Methods: The chromatographic separation was performed on Water’s 2695(Alliance) equipped with a photodiode array detector at 300 nm. The method was developed on Discovery C18 column (250×4.6, 5 mm) using orthophosphoric acid and acetonitrile (55:45 % v/v) with the flow rate of 1 ml/min at 30°C. The degradation studies of simeprevir were carried out under the stress conditions of hydrolysis (acid, base, and neutral), oxidation, photolytic, and thermal as per the International Conference on Harmonization (ICH) guidelines. The peroxide hydrolysis shows more critical impurities which were well resolved from pure drug with the application of design of experiment and optimized the method. Results: Independent variables (critical analytical attributes) selected for the method optimization were mobile phase ratio, flow rate, and temperature of the column based on the risk assessment. The retention time and resolution were selected as the method response. In response surface method, the central composite design and 23 factorial designs were employed for the optimization of the method. The polynomial equation was derived for the estimation of method response. Conclusion: The method was optimized for better resolution among the drug, and impurity peaks were then validated as per the ICH parameters.

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