Isolation and characterization of urolithin b from asphaltum (original) (raw)

Quality Control: Curb Counterfeiting of Asphaltum (Shilajit)

2018

Increased demand of Asphaltum (Shilajit) in immunity modulation and fertility has generated intense interest among the producers and regulators to ensure its quality. For doing so, there is a need to isolate its chemical markers and analyze the same. Urolithins (Benzocoumarins) are one of the bioactive phytoconstituents in Asphaltum. Urolithin A and B are found to be present in Shilajit. The objective of this study was to develop a simple method for isolation of Urolithin A and B from Asphaltum. Elementary solvent partitioning technique was used for the extraction and isolation of Urolithins. Organic solvents like Methanol, Ethyl acetate, Petroleum ether etc were used. The isolated compounds were identified and characterized by TLC (Thin Layer Chromatography), UV (Ultra-violet), IR (Infrared) and MS (Mass) spectral analysis and purity was confirmed by HPLC (High Performance Liquid Chromatography) analysis. The isolated markers Urolithin A shows absorption maxima at 280, retention fa...

Substantiation of technological parameters of the oil extract obtained from Urtica dioica roots based on the yield determination of phytosterols using capillary gas chromatography method

ScienceRise: Pharmaceutical Science, 2021

Due to the content of phytosterols, extractive preparations of Urtica dioica roots are able to show antiandrogenic effect in the case of external therapy of men and women with androgenic alopecia. Oil extracts (OE) are characterized by several advantages when applied to the skin of the scalp compared to water-alcohol extracts. For the development of OE technology from Urtica dioica roots, it is important to choose the optimal extraction parameters, which are based on the quantitative determination of phytosterols in the extractant and the studied samples of extracts. The aim of the work is to choose the optimal parameters for obtaining OE from Urtica dioica roots based on quantitative determination of phytosterols content in experimental samples of OE by gas capillary chromatography. Materials and methods. Objects of the research – Urtica dioica root, refined corn oil, refined sunflower oil, samples of oil extracts. Determination of phytosterol content in experimental samples was ca...

COMPARISON OF THREE EXTRACTION METHODS OF ALLOPURINOL IN URIC ACID HERBAL MEDICINE WITH HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY QUANTIFICATION Original Article

International Journal of Applied Pharmaceutics, 2021

Objective: This study was aimed to understand and determine the effectiveness of allopurinol extraction in herbal medicine from three extraction methods based on parameters of accuracy and precision. Methods: The study consisted of three methods including dissolving and filtering, liquid-liquid extraction, and solid-phase extraction with mixedmode cation exchanger (SPE-MCX). The procedures were carried out using NaOH and HCl in dissolving and filtering method; methanol, HCl, and ethyl acetate in liquid-liquid extraction; and NH4OH elution solvent in SPE-MCX. Results: The results showed that extraction effectiveness based on accuracy level was the dissolving and filtering method>SPE-MCX>liquid-liquid extraction with % recovery+SD of 91.314+2.903%, 87.533+4.950%, and 54.549+3.517%, respectively. The precision level was the dissolution and filtering method>SPE-MCX>liquid-liquid extraction based on % relative standard deviations (RSD) of 3.18%, 5.226%, and 6.446%, respectively. Conclusion: It can be concluded that the allopurinol extraction method with the highest effectiveness based on accuracy and precision parameters in herbal medicine is the dissolving and filtering method.

Development and Validation of a Stability-Indicating Method for the Estimation of Ursodeoxycholic Acid using the RP-HPLC method

International Journal of Scientific Research in Chemistry, 2020

Given that currently published analytical methods of ursodeoxycholic acid (UDCA) involve complex procedures and equipment, the purpose of this paper was to present the validation of a simple, rapid, accurate and precise isocratic UV and stability indicating RP-HPLC method for quantification residual solvents of ursodeoxycholic acid. Such a method would be critical in prospective developers. Validated method demonstrated Ursodeoxycholic acid separation without interference from the solvents with the most relevance for developing of tablet pharmaceutical drug carries. Method was linear over studied Ursodeoxycholic acid concentration range (2-10 µg/mL) with acceptable precision and accuracy. Method validation is carried out by using linearity (regression coefficient =0.934), accuracy (96.08 to 98.25), precision (intraday= % R.S.D. – 0.98and interday = % R.S.D. - 1.52), LOD (0.1) and LOQ (0.303), robustness (change in flow rate, change in wavelength and mobile phase composition was found to be 3.383 ± 3.47 respectively). Development and validation of Ursodeoxycholic acid was successfully carried out by using UV and HPLC method.

Estimation of Levodopa in the Unani Drug Mucuna pruriens Bak. and Its Marketed Formulation by High-Performance Thin-Layer Chromatographic Technique

Journal of AOAC INTERNATIONAL, 2019

Background: Mucuna pruriens Bak. Syn. Mucuna prurita Hook. seed is the rich source of levodopa (L-dopa) and has been used in traditional medicines to treat diseases resembling Parkinson’s disease. Objective: In the present study, a new HPTLC method was developed and validated for estimation of L-dopa from M. pruriens (black- and white-colored seeds) collected from two different locations in India. Method: TLC aluminum plates precoated with silica gel were used as the stationary phase. The plates were developed to a distance of 60 mm at a temperature of 22 ± 4°C in a twin glass chamber saturated with ethyl acetate–methanol–formic acid–water (15+3+3+4.5, v/v/v/v), as the mobile phase. Results: The Rf value of L-dopa was found to be 0.45. L-dopa was quantified at 282 nm, the wavelength of maximum absorbance by a densitometric scanner. The TLC plate was derivatized by ninhydrin reagent and photodocumented. L-dopa showed a good linearity in the concentration range 400–1000 ng/spot. The l...

LC-MS/MS Method Applied to the Detection and Quantification of Ursodeoxycholic Acid Related Substances in Raw Material and Pharmaceutical Formulation

Journal of Pharmacy and Pharmacology 6 (2018) 448-455, 2018

Objective: To develop a highly sensitive LC-MS/MS (liquid chromatography-mass spectrometry/mass spectrometry) method applied to the detection and quantitation of UDCA (ursodeoxycholic acid) related substances such as CA (cholic acid), DCA (deoxycholic acid), CDCA (chenodeoxycholic acid) and LCA (lithocholic acid) in raw material and pharmaceutical formulation. Methods: The method was validated for specificity, linearity, accuracy, precision, robustness. A triple quadrupole mass detector was employed, equipped with an ESI (electrospray ionization) source operated in the negative ion mode. The chromatographic system consisted of a Symmetry C18 column (150 mm × 4.6 mm, id; particle size 5 µm) and methanol-acetonitrile-ammonium acetate (pH 7.6; 10 mM) (40:40:20, v/v/v) as the mobile phase. The chromatographic conditions were 25 uL injection volume, flow rate of 0.4 mL/min and column temperature set at 35 °C. Key findings: The method requires a minimum sample amount and presents very low LOD (limits of detection) for CA (0.29 ng/mL), DCA (0.59 ng/mL), CDCA (0.13 ng/mL) and LCA (0.44 ng/mL) in comparison to LC methods coupled to different detectors like UV (ultraviolet), fluorescence and refractive index. Conclusions: The developed and validated LC-MS/MS method for the determination of UDCA and related substances in raw material and in a suspension was advantageous since it required a minimum sample amount. In turn, it could be used as a stability indicating method.

Journal of Chromatography & Separation Techniques

2022

Objective: The objective of present work is to develop and validate HPTLC method for simultaneous estimation of Curcumin and Azadirachtin in marketed formulation Materials and methods: HPTLC method was developed using a solvent system Toluene: Ethyl acetate: Ammonia: Formic acid (4:3:2.5:0.5 v/v/v/v) using a stationary phase Silica Gel 60 F254 and the saturation time is 15 min. The developed method was standardized in terms of validation parameters such as specificity, linear range, precision, robustness, ruggedness and reproducibility as per ICH guidelines. Newly developed and validated method was successfully applied for estimation of Curcumin and Azadirachtin in marketed formulation. Results: The linearity range for the both Curcumin and Azadirachtin was found to be 1.5-15 µl/spot. The limit of detection found to be 0.383213 µl/spot for the Curcumin and 0.46572 µl/spot for Azadirachtin. The limit of quantification is found to be 1.16125 µl/spot for the Curcumin and 1.411272 µl/spot for Azadirachtin. Recovery of Azadirachtin in marketed formulation was observed in the range of 91%-109% and recovery of Curcumin in marketed formulation was observed in the range of 91%-105%. All the precision and repeatability results were within acceptance range less than 2%. Assay of Curcumin and Azadirachtin was found to be 92.95% and 91.79% respectively. The Rf value of Curcumin is found to be 0.5 ± 0.03 and the Rf value of Azadirachtin is found to be 0.57 ± 0.04. Conclusion: The method was found to be simple, accurate, environment friendly, reproducible and can be used for routine estimation analysis of Curcumin and Azadirachtin in marketed formulation.