Extraction Optimization for Phenolic- and Withanolide-Rich Fractions from Withania somnifera Roots: Identification and Quantification of Withaferin A, 12-Deoxywithastromonolide, and Withanolide A in Plant Materials and Marketed Formulations Using a Reversed-Phase HPLC–Photodiode Array Detection Method

2018 ◽  
Vol 101 (6) ◽  
pp. 1773-1780 ◽  
Author(s):  
Satyanshu Kumar ◽  
Raghuraj Singh ◽  
Narendra Gajbhiye ◽  
Tushar Dhanani
Keyword(s):  
Withania Somnifera ◽  
Phenolic Content ◽  
Hplc Method ◽  
Withaferin A ◽  
Total Phenolic ◽  
Photodiode Array Detection ◽  
Withanolide A ◽  
Photodiode Array ◽  
Array Detection ◽  
Identification And Quantification

Abstract Background: Both the roots and leaves of Withania somnifera are products of commerce. They contain active compounds of therapeutic value and mostly different withanolides. Several pharmacological activities of W. somnifera have links to one or more withanolides. The presence of phenolic compounds in extracts could play a vital role in the reduction of blood glucose levels in diabetic subjects. Objective: The present study was carried out for the selection of a solvent to prepare extracts rich in phenolics, withaferin A (WA), 12-deoxywithastromonolide (12WD), and withanolide A (WDA). A simple, rapid HPLC method was also developed for the identification and quantification of WA, 12WD, and WDA. Methods: The extraction efficiency of aqueous alcoholic solvents including hexane, chloroform, ethyl acetate, and methanol were compared for three selected withanolides and total phenolic content. The contents of WA, 12WD, and WDA and total phenolics were determined in the extracts. The quality of nine formulations containing W. sominfera were also compared in terms of the content of WA, 12WD, and WDA and total phenolics. Results: The maximum extract yield and the total withanolide and phenolic content were obtained from aqueous alcoholic compositions at 50:50 (v/v), 70:30 (v/v), and 100:0 (v/v), respectively. In the case of organic solvents, chloroform and ethyl acetate yielded the highest concentrations of phenolics and three withanolides, respectively. The total phenolic content in formulations was in the range of 1.84–3.13%, and total withanolide content showed wide variability. Conclusions: The outcome of the present investigation could be utilized for the selection of extraction solvents to prepare W. somnifera–enriched extracts and their quality monitoring by using the developed and validated HPLC-Photodiode array detection method. Highlights: A process for preparation of phenolics and withanolides (withaferin A, 12-deoxywithastramonolide and withanolide A) enriched extracts of Withania somnifera. Simple and rapid HPLC method was also developed and validated as per the ICH guidelines for identification and quantification of three major withanolides. The developed HPLC method was applied to analyze the quality of extracts and marketed herbal products (mono, as well as poly constituents). Optimized extraction process could be utilized for upscaling process development in preparation of enriched extracts from Withania somnifera, crop improvement, bio-prospection studies and quality control.

scholarly journals Quantitative Determination of Pregnanes from Aerial Parts of Caralluma Species Using HPLC-UV and Identification by LC-ESI-TOF

2011 ◽  
Vol 94 (5) ◽  
pp. 1383-1390
Author(s):  
Bharathi Avula ◽  
Yatin J Shukla ◽  
Yan-Hong Wang ◽  
Ikhlas A Khan
Keyword(s):  
Quantitative Determination ◽  
Dietary Supplements ◽  
Hplc Method ◽  
Photodiode Array Detection ◽  
Plant Materials ◽  
Aerial Parts ◽  
Photodiode Array ◽  
Array Detection ◽  
Na Ions

Abstract An HPLC method was developed for the quantitative determination of five pregnane derivatives from aerial parts of Caralluma species and dietary supplements. The method was validated for linearity, repeatability, LOD, and LOQ. The LOD and LOQ of five pregnane compounds were found to be in the range of 1–5 and 3–15 μg/mL, respectively, by HPLC using photodiode array detection. This method was applied to the identification of three plant materials of Caralluma species (C. fimbriata, C. umbellate, and C. attentuata) and seven dietary supplements claiming to contain C. fimbriata. An LC/MS coupled with electrospray ionization interface method was used for the identification of compounds and involved the use of [M+Na]+ ions in the positive ion mode with extracted ion chromatogram.

scholarly journals Simultaneous HPLC Determination of Three Bioactive Alkaloids in the Asian Medicinal Plant Stephania rotunda

2010 ◽  
Vol 5 (6) ◽  
pp. 1934578X1000500 ◽  
Author(s):  
Sothavireak Bory ◽  
Sok-Siya Bun ◽  
Béatrice Baghdikian ◽  
Fathi Mabrouki ◽  
Sun Kaing Cheng ◽  
...  
Keyword(s):  
High Performance ◽  
Potassium Phosphate ◽  
Solvent System ◽  
Hplc Method ◽  
Photodiode Array Detection ◽  
Linear Behavior ◽  
Photodiode Array ◽  
Array Detection ◽  
The Mean

A reliable high-performance liquid chromatography (HPLC) method coupled with photodiode array detection has been developed and validated for the determination of three major alkaloids: cepharanthine, tetrahydropalmatine and xylopinine in Stephania rotunda Lour. (Menispermaceae) collected in Cambodia. The chromatographic separation was carried out on a Symmetry C8 column (250 mm x 4.6 mm, 5 μm, Waters), with an isocratic solvent system of 25 mM potassium phosphate buffer (pH 3.5) – acetonitrile. UV detection was performed at 282 nm. Good linear behavior over the investigated concentration ranges was observed with values of r2>0.9964 for all the analytes. The method was reproducible with intra- and inter-day variations of less than 3.91%. The mean recoveries of the analytes ranged from 95.7 to 104.6%. The proposed method was linear, accurate, precise and specific. The validated method was successfully applied to quantify the three alkaloids in various parts of Stephania rotunda and in tubers collected from different Cambodian regions. The results indicated that the developed HPLC method could be used for the quality control of S. rotunda.

scholarly journals Development and Validation of an RP-HPLC-PDA Method for Determination of Paracetamol, Caffeine and Tramadol Hydrochloride in Pharmaceutical Formulations

2021 ◽  
Vol 14 (5) ◽  
pp. 466
Author(s):  
Fernando J. Pereira ◽  
Aida Rodríguez-Cordero ◽  
Roberto López ◽  
Luis C. Robles ◽  
A. Javier Aller
Keyword(s):  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Fluorescence Detector ◽  
Photodiode Array Detection ◽  
Tramadol Hydrochloride ◽  
Rp Hplc ◽  
Photodiode Array ◽  
Array Detection ◽  
Tablet Dosage

Paracetamol (acetaminophen) (PAR), caffeine (CAF) and tramadol hydrochloride (TRA) are important drugs widely used for many clinical purposes. Determination of their contents is of the paramount interest. In this respect, a quick, simple and sensitive isocratic RP-HPLC method with photodiode array detection was developed for the determination of paracetamol, caffeine and tramadol in pharmaceutical formulations. An improved sensitive procedure was also evolved for tramadol using a fluorescence detector system. A C18 column and a mobile phase constituted by methanol/phosphate were used. LODs were found to be 0.2 μg/mL, 0.1 μg/mL and 0.3 μg/mL for paracetamol, caffeine and tramadol hydrochloride, respectively, using photodiode-array detection. Alternatively, LOD for tramadol decreased to 0.1 μg/mL with the fluorescence detector. Other notable analytical figures of merit include the linear concentration ranges, 0.8–270 μg/mL, 0.4–250 μg/mL and 1.0–300 (0.2–40) μg/mL, for the same ordered analytes (including the fluorescence detector). The proposed method was successfully applied for the quantitative determination of the three drugs in tablet dosage forms.

STABILITY INDICATING RP-HPLC METHOD FOR SIMULTANEOUS ESTIMATION OF SIMETHICONE, DOMPERIDONE, MAGALDRATE AND SODIUM ALGINATE: APPLICATION TO SYRUP FORMULATION

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (11) ◽  
pp. 42-52
Author(s):  
Pulagurtha Bhaskararao ◽  
Gowri S. Dannana ◽  
Keyword(s):  
Sodium Alginate ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Photodiode Array Detection ◽  
Stability Indicating ◽  
Rp Hplc ◽  
Relative Standard ◽  
Peak Areas ◽  
Photodiode Array ◽  
Array Detection

A rapid and validated stability indicating RP-HPLC method using isocratic elution and coupled with photodiode array detection was developed for quantifying the content of simethicone, domperidone, magaldrate and sodium alginate in bulk and syrup formulation. The best mobile phase used in this study consisted of 0.1 % orthophosphoric acid/acetonitrile (50/50, V/V) with a flow rate of 0.7 mL min-1. Under optimized conditions used in this study, selected drugs were eluted at 3.301 min (simethicone), 4.293 min (domperidone), 5.220 min (magaldrate) and 6.149 min (sodium alginate) within 12 min run time without any interfering excipients. Peak areas and selected drug content demonstrated excellent linearity (simethicone – 5 to 30 µg mL-1; domiperidone – 2.5 to 15 µg mL-1; magaldrate – 120 to 720 µg mL-1; sodium alginate – 25 to 150 µg mL-1). Percent recovery, which represents accuracy, was 99.12–100.18 % for simethicone, 99.59-100.52 % for domperidone, 99.23-100.25 % for magaldrate and 99.57-100.02 % for sodium alginate. Percent relative standard deviation, which represents precision, was observed in the range of 0.078-0.983 % (simethicone), 0.528-0.861 % (domperidone), 0.278-1.069 % (magaldrate), 0.316-0.572 % (sodium alginate). The developed method displayed favourable accuracy and recovery and was suitable for determining the content of simethicone, domperidone, magaldrate and sodium alginate combination in syrup formulations.

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