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 ◽  
...  

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.

Planta Medica ◽  
2020 ◽  
Author(s):  
Omer I. Fantoukh ◽  
Yan-Hong Wang ◽  
Abidah Parveen ◽  
Mohammed F. Hawwal ◽  
Gadah A. Al-Hamoud ◽  
...  

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.


2019 ◽  
Vol 2019 ◽  
pp. 1-15 ◽  
Author(s):  
Yongsong Xu ◽  
Sha Wu ◽  
Yanchuan Wu ◽  
Muxin Gong ◽  
Zhimin Wang

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.


Antioxidants ◽  
2020 ◽  
Vol 9 (6) ◽  
pp. 488
Author(s):  
Agnieszka Szopa ◽  
Michał Dziurka ◽  
Sebastian Granica ◽  
Marta Klimek-Szczykutowicz ◽  
Paweł Kubica ◽  
...  

Schisandra rubriflora is a dioecious, underestimated medicinal plant species known from traditional Chinese medicine. The present study was aimed at characterising the polyphenolic profile composition and the related antioxidant capacity of S. rubriflora fruit, stem and leaf and in vitro microshoot culture extracts. Separate analyses of material from female and male specimens were carried out. This study was specifically aimed at detailed characterisation of the contribution of phenolic compounds to overall antioxidant activity using ultra-high-performance liquid chromatography with a photodiode array detector coupled to electrospray ionization ion trap mass spectrometry (UHPLC-DAD-ESI-MS3) and a high-performance liquid chromatography-diode array detector (HPLC-DAD). Using UHPLC-DAD-ESI-MS3, twenty-seven phenolic compounds from among phenolic acids and flavonoids were identified. Concentrations of three phenolic acids (neochlorogenic, chlorogenic and cryptochlorogenic acids) and eight flavonoids (hyperoside, rutoside, isoquercitrin, guaijaverin, trifolin, quercetin, kaempferol, and isorhamnetin) were determined using HPLC-DAD using reference standards. The highest total phenolic content was confirmed for the stem and leaf extracts collected in spring. The contents of phenolic compounds of in vitro biomasses were comparable to that in the fruit extracts. The methanolic extracts from the studied plant materials were evaluated for their antioxidant properties using various in vitro assays, namely free radicals scavenging estimation using 2,2-diphenyl-1-picryl-hydrazyl-hydrate (DPPH), ferric-reducing antioxidant power (FRAP) and cupric-reducing antioxidant capacity (CUPRAC) as well as QUick, Easy, New, CHEap, and Reproducible CUPRAC (QUENCHER-CUPRAC) assays. A close relationship between the content of polyphenolic compounds in S. rubriflora and their antioxidant potential has been documented.


Author(s):  
ADRIANA YURIKO KOGA ◽  
BRUNA CARLETTO ◽  
LEANDRO CAVALCANTE LIPINSKI ◽  
TRAUDI KLEIN ◽  
PAULO VITOR FARAGO

Objective: A simple high-performace liquid chromatography method was developed and validated to determine 17-β estradiol in poly (ε-caprolactone) nanocapsules. Methods: The chromatographic conditions were as follows: C18 GL column with a mobile phase of acetonitrile:water (92:8 v/v) at flow rate of 1.5 mL/min with detection at 280 nm. The evaluated parameters were specificity, linearity, limits of detection and quantification, precision, accuracy, and robustness. Results: The method was specific and linear (r=0.9982). The limits of detection and quantification were 5.78 μg.mL-1 and 17.54 μg.mL-1, respectively. Suitable accurancy and robustness were obtained. The stability assay showed that pH variation occured after 120 days of storage, and no changes were observed regarding the size and polydispersion parameters. The applicability of the method was evaluated by determining the encapsulation efficiency of the E2 nanocapsules after 120 days of storage. The results showed values >99%. Conclusion: The results demonstrated the applicability of the developed and validated analytical method.


2018 ◽  
Vol 10 (1) ◽  
pp. 133
Author(s):  
Dwi Karina Natalia ◽  
Harmita . ◽  
Taufiq Indra Rukmana

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.


2014 ◽  
Vol 68 (7) ◽  
Author(s):  
Joanna Ronowicz ◽  
Bogumiła Kupcewicz ◽  
Łukasz Pałkowski ◽  
Piotr Bilski ◽  
Tomasz Siódmiak ◽  
...  

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.


2021 ◽  
Vol 49 (2) ◽  
pp. 12394
Author(s):  
Constantinos SALIS ◽  
Ioannis E. PAPADAKIS ◽  
Marianna HAGIDIMITRIOU

Mediterranean diet is almost synonymous to the healthy lifestyle and diet nowadays. Some of the major components of the diet are the products of the olive tree, fruits and olive oil, which are classified as medical foods, due to their nutraceutical benefits and their protective properties against cancer, cardiovascular diseases, age-related diseases, neurodegenerative disorders and other diseases. The key contributors to these properties are the phenolic compounds such as hydroxytyrosol, tyrosol and oleuropein. Table olives are being processed with several methods in order to reduce the bitterness of the olive fruit and the impact of the processing on phenolic compounds has not been studied extensively. In the present study, changes in the concentration of the most important phenolic compounds were quantified in fresh, Greek-style and Spanish-style processed olive fruits of cv. ‘Kalamata’, using two different analytical methods for identification and quantification: high-performance liquid chromatography diode array detector (HPLC-DAD) and ultrahigh-performance liquid chromatography tandem mass spectrometry (LC-(ESI)-MS/MS). The phenolic compounds that were identified and quantified were hydroxytyrosol, tyrosol, verbascocide, rutin, oleuropein and luteolin. Both processing methods used altered the phenolic compounds concentration in ‘Kalamata’ olive fruits compared to untreated fruits. In both analytical methods, a statistically significant increase in verbascoside and hydroxytyrosol concentration and a statistically significant decrease in rutin concentration was observed in both, Greek-style and Spanish-style, processed olive fruits.


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