scholarly journals Chromatographic Methods for the Determination of Primula Acid 1 Content in Primulae extractum fluidum

2020 ◽  
Keyword(s):  
Calibration Curve ◽  
Mobile Phase ◽  
Active Component ◽  
Reversed Phase ◽  
Hplc Method ◽  
Reversed Phase Chromatography ◽  
Triterpenoid Saponins ◽  
Simple Preparation ◽  
Primula Veris

Primula veris L. (Primulaceae)is healing plant, whose root is officially used to treat cough associated with cold. Other reported indications are respiratory, thoracic and mediastinal disorders. These effects are result of high contents of triterpenoid saponins and phenolic glycosides. Primula acid 1 (PA 1, also primulasaponin 1) is main active component in Primula elatior L. This paper presents an optimized high pressure liquid chromatography (HPLC) method for the determination of primula acid 1 content in Primulae extractum fluidum. TLC was performed to check for the presence of the substance of interest. The determination was performed by reversed phase chromatography using C18 as a stationary phase. The mobile phase used for separation consisted of 0.2% H3PO4 and acetonitrile. This method was validated through different parameters. The detection limit for primula acid 1 was LD=10.41 µg/ml, and the quantification limitwas LQ=34.69 µg/ml. In order to determine the content of primula acid 1, a calibration curve was constructed, and the content of primula acid 1 was calculated by the equation of the calibration curve and was 0.2793 mg per gram of extract. The results and simple preparation of sample show that HPLC is the method of choice for this type of analysis.

scholarly journals Simultaneous Determination of Preservatives (Methyl Paraben and Propyl Paraben) in Sucralfate Suspension Using High Performance Liquid Chromatography

2011 ◽  
Vol 8 (1) ◽  
pp. 340-346 ◽  
Author(s):  
Rajesh M. Kashid ◽  
Santosh G. Singh ◽  
Shrawan Singh
Keyword(s):  
High Performance Liquid Chromatography ◽  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Reversed Phase Hplc ◽  
Methyl Paraben ◽  
Propyl Paraben

A reversed phase HPLC method that allows the separation and simultaneous determination of the preservatives methyl paraben (M.P.) and propyl paraben (P.P.) is described. The separations were effected by using an initial mobile phase of water: acetonitrile (50:50) on Inertsil C18 to elute P.P. and M.P. The detector wavelength was set at 205 nm. Under these conditions, separation of the two components was achieved in less than 10 min. Analytical characteristics of the separation such as precision, specificity, linear range and reproducibility were evaluated. The developed method was applied for the determination of preservative M.P. and P.P. at concentration of 0.01 mg/mL and 0.1 mg/mL respectively. The method was successfully used for determining both compounds in sucralfate suspension.

VALIDATED RP-HPLC METHOD FOR DETERMINATION OF ENZALUTAMIDE IN BULK DRUG AND PHARMACEUTICAL DOSAGE FORM

INDIAN DRUGS ◽  
2016 ◽  
Vol 53 (11) ◽  
pp. 46-50
Author(s):  
Z. G Khan ◽  
◽  
S. S. Patil ◽  
P. K. Deshmukh ◽  
P. O. Patil
Keyword(s):  
Retention Time ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Uv Detector ◽  
Chromatography Method ◽  
Pharmaceutical Dosage Form ◽  
Bulk Drug

Novel, isocratic reversed phase high performance liquid chromatography method was developed and validated for the determination of enzalutamide (EZA) in bulk drug and pharmaceutical formulation. Efficient separation was achieved on PrincetonSPHER C18 100A, 5μ (250×4.6 mm) under the isocratic mode of elution using acetonitrile: water (80:20) % V/V as a mobile phase pumped in to the column at flow rate 1.0 mL/min. The effluent was monitored at 237.0 nm using UV detector. EZA was eluted in the given mobile phase at retention time (tR) of 3.2 minutes. The standard calibration curve was linear over the concentration range 10 - 60 μg/mL with correlation coefficient 0.997. The method was validated for accuracy, precision, sensitivity, robustness, ruggedness and all the resulting data treated statistically. The system suitability parameters like retention time, theoretical plates, tailing factor, capacity factor were found within the limit.

scholarly journals Development and validation of a reversed-phase HPLC method for determination of assay content of Teriflunomide by the aid of BOMD simulations

2021 ◽  
pp. 281-294 ◽  
Author(s):  
Abolghasem Beheshti ◽  
Zahra Kamalzadeha ◽  
Monireh Haj-Maleka ◽  
Meghdad Payaba ◽  
Mohammad Amin Rezvanfar ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Potassium Dihydrogen Phosphate ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Dihydrogen Phosphate ◽  
Td Dft ◽  
High Level ◽  
Development And Validation

Due to the new hopes for treatment of multiple sclerosis (MS) diseases by Teriflunomide (TFN), in this project, a cheap, robust, and fully validated method has been developed both for determination of assay content in API (active pharmaceutical ingredient), and for related impurities analysis (RIA). To operate the method, a common C18, end-capped (250 × 4.6) mm, 5µm liquid chromatography column, was applied. The mobile phase A was prepared by dissolving 2.74 g (20mM) of PDP (potassium dihydrogen phosphate) and 3.72 g (50mM) of PC (potassium chloride) in water (1000 mL). Then, pH was adjusted to 3.0 by adding OPA (ortho-phosphoric acid) 85%; while, the mobile phase B was acetonitrile (ACN) (100%). In order to confirm the experimental data about the λmax of TFN, we have used the Born-Oppenheimer molecular dynamics (BOMD) simulations, quantum mechanics (QM), and TD-DFT calculations. According to the results, the method showed a high level of suitability, specificity, linearity, accuracy, precision, repeatability, robustness, and reliable detection limit.

scholarly journals DEVELOPMENT AND VALIDATION OF A HIGH PERFORMANCE LIQUID CHROMATOGRAPHIC METHOD DETERMINATION OF ZIDOVUDINE ENCAPSULATED IN PCL NANOPARTICLES

2017 ◽  
Vol 1 (2) ◽  
pp. 1-8
Author(s):  
Milena Cristina Ribeiro Souza Magalhães ◽  
Alisson Samuel Portes Caldeira ◽  
Hanna De Sousa Rocha Almeida ◽  
Sílvia Ligório Fialho ◽  
Armando Da Silva Cunha Junior
Keyword(s):  
Mobile Phase ◽  
High Performance ◽  
High Performance Liquid Chromatographic ◽  
Reversed Phase ◽  
Hplc Method ◽  
Liquid Chromatographic Method ◽  
Development And Validation ◽  
Liquid Chromatographic ◽  
Isocratic Mode

A reversed-phase high-performance liquid chromatographic (HPLC) method was developed and validated for the determination of encapsulation efficiency of zidovudine in nanoparticules. The method was carried out in isocratic mode using 0.040M sodium acetate: methanol: acetonitrile: glacial acetic acid (880:100:20:2) as mobile phase, a C8 column at 25ºC and UV detection at 240 nm. The method was linear (r2 ˃ 0.99) over the range of 25.0-150.0 μg/mL, precise (RSD ˂ 5%), accurate (recovery = 100.5%), robust and selective. The validated HPLC-UV method can be successfully applied to determine the rate of zidovudine in nanoparticules.

Quantitation of Transdermal Tadalafil in Human Skin by Reversed-Phase High-Performance Liquid Chromatography

2012 ◽  
Vol 95 (4) ◽  
pp. 1064-1068 ◽  
Author(s):  
Mohammed H Mehanna ◽  
Abdel M Motawaa ◽  
Magda W Samaha
Keyword(s):  
High Performance Liquid Chromatography ◽  
Liquid Chromatography ◽  
Human Skin ◽  
Mobile Phase ◽  
High Performance ◽  
Reversed Phase ◽  
Hplc Method ◽  
Drug Deposition ◽  
Transdermal Permeation

Abstract A reliable and sensitive HPLC method was developed for the quantitation of tadalafil transdermal permeation through human skin. An RP column with UV detection at 290 nm was used for chromatographic separation at ambient temperature. The mobile phase was acetonitrile–water containing 20 mM pH 7 phosphate buffer (35/65, v/v) with a flow rate of 1.0 mL/min. The LOQ achieved was 1 ng/mL, and the calibration curve showed good linearity over the concentration range of 5–2000 ng/mL for tadalafil, with a determination coefficient (R2) of 0.998. The RSD values of intraday and interday analyses were all within 7%. Parameters of validation proved the precision of the method; this validated method was applied for the determination of tadalafil in transdermal permeation and drug deposition in human skin studies.

scholarly journals Determination of urinary free cortisol by HPLC

1997 ◽  
Vol 43 (8) ◽  
pp. 1386-1391 ◽  
Author(s):  
Ursula Turpeinen ◽  
Helene Markkanen ◽  
Matti Välimäki ◽  
Ulf-Håkan Stenman
Keyword(s):  
Solid Phase Extraction ◽  
Mobile Phase ◽  
Solid Phase ◽  
Internal Standard ◽  
Reversed Phase ◽  
Hplc Method ◽  
Extraction Column ◽  
Phase Extraction ◽  
Free Cortisol

Abstract We here report a reversed-phase HPLC method for the determination of free cortisol in human urine, using methylprednisolone as the internal standard. Before chromatography, samples were extracted with a C18 solid-phase extraction column and the steroids were separated on a LiChrospher 100 C18 column with a mobile phase of methanol/acetonitrile/water (43/3/54 by vol). Linearity, precision, and accuracy of the method were established. The detection limit was 10 pmol of cortisol, and total CVs were <8%. With various solid-phase extraction columns the recovery of cortisol was 36–97%; recovery of the internal standard was 43–85%. Study of interference by 6 other steroids and metabolites and 24 drugs showed that carbamazepine and digoxin partly overlapped with cortisol, but this interference could be reduced by modification of the mobile phase. The HPLC method was compared with an RIA and an automated immunoassay method. The results obtained by HPLC averaged 40% of the RIA values.

Development and Validation of a Reversed-Phase HPLC Method for Determination of Alkaloids from Papaver somniferum L. (Papaveraceae)

2012 ◽  
Vol 95 (2) ◽  
pp. 399-405 ◽  
Author(s):  
Jelena Acevska ◽  
Aneta Dimitrovska ◽  
Gjoshe Stefkov ◽  
Katerina Brezovska ◽  
Marija Karapandzova ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Ph Value ◽  
Reversed Phase ◽  
Hplc Method ◽  
Papaver Somniferum ◽  
Chromatographic Behavior ◽  
Organic Modifier ◽  
Column Temperature ◽  
Development And Validation

Abstract An HPLC method for the separation of six target alkaloids from Papaver somniferum L. (morphine, codeine, oripavine, thebaine, papaverine, and noscapine) was developed, optimized, and validated. The chromatographic behavior of these alkaloids was investigated using a reversed-phase chromatography at acidic and alkaline pH. The effects of ion-pairing agents, pH value of the mobile phase, concentration of the buffer components, mobile phase organic modifier, and column temperature were studied. Regardless of the large differences in their pKa values, all alkaloids were separated within a close retention window, and good peak shape was achieved for each of the six alkaloids. The proposed method has adequate selectivity, linearity, accuracy, precision, and reproducibility and is applicable for poppy straw.

scholarly journals Stability Indicating HPLC Method for the Determination of Delamanid in Pharmaceutical Dosage Form

2021 ◽  
Vol 11 (1-s) ◽  
pp. 108-112
Author(s):  
Advaita B. Patel ◽  
Deepa R. Patel ◽  
Dhaval M. Patel ◽  
Mansi Babaria
Keyword(s):  
Analytical Method ◽  
Mobile Phase ◽  
Dosage Form ◽  
Degradation Products ◽  
Stress Test ◽  
Reversed Phase ◽  
Hplc Method ◽  
Pharmaceutical Dosage Form ◽  
Stability Indicating

Delamanid is successfully used for treatment of MDR TB. A stability indicating analytical method has been developed and validated. In this study Delamanid was degraded under different stress test conditions as per International Conference on Harmonization. The degraded samples were used to develop a stability-indicating high performance liquid chromatographic (HPLC) method for the Delamanid. The Delamanid was well separated from degradation products using a reversed-phase Hypersil BDS C18 (250 mm × 4.6mm i.d., 5µm) column and a mobile phase comprising of 0.01M pH 2.70 Phosphate Buffer: Acetonitrile (pH 3.50) 70:30, pH of mobile phase was adjusted with Glacial acetic acid and other HPLC parameters were flow rate 1 mL/min, detection wavelength 254 nm and injection volume 10 µl. The method was validated for linearity, precision, accuracy, ruggedness and robustness. Results obtained after validation study indicating that the proposed single method allowed analysis of Delamanid in the presence of their degradation products formed under a variety of stress conditions. The developed procedure was also applicable to the determination of stability of the Delamanid in commercial pharmaceutical dosage form. Keywords:  Delamanid, stability indicating analytical method, HPLC

scholarly journals A simple isocratic RP-HPLC method for quality control of oseltamivir capsules

2012 ◽  
Vol 31 (2) ◽  
pp. 205
Author(s):  
Agim Ameti ◽  
Jasmina Slavkovska ◽  
Katerina Starkoska ◽  
Zorica Arsova-Sarafinovska
Keyword(s):  
Mobile Phase ◽  
Limit Of Detection ◽  
Degradation Products ◽  
Reversed Phase ◽  
Hplc Method ◽  
Sample Treatment ◽  
Limit Of Quantification ◽  
Elution Time ◽  
Rp Hplc

A simple isocratic reversed-phase high performance liquid chromatographic (RP-HPLC) method was developed for determination of oseltamivir active pharmaceutical ingredient (API) in bulk drug and pharmaceuticals. The separation was achieved on a Purospher STAR® RP – 18e column with a mobile phase consisting of methanol- 0.02 mol l-1 phosphate buffer, pH 5, 50:50 (v/v). Chromatographic results demonstrated the specificity of the method for determination of oseltamivir in presence of degradation products generated in studies of forced decomposition. The limit of detection (LOD) and limit of quantification (LOQ) for oseltamivir phosphate were 0,0162 μg ml-1 and 0,0491 μg ml-1, respectively. The advantages of this method include simple sample treatment and short elution time (less than 6 min). Furthermore, using methanol instead of acetonitrile in a mobile phase composition considerably reduces the laboratory expenses, still retaining adequate sensitivity for routine analysis as well as for evaluation of potentially counterfeit Tamiflu® products. 

scholarly journals Development and Validation of an HPLC Method for the Determination of the macrolide antibiotic Clarithromycin using Evaporative Light Scattering Detector in raw materials and Pharmaceutical Formulations

2017 ◽  
Vol 6 (4) ◽  
pp. 133-141 ◽  
Author(s):  
Zampia Tzouganaki ◽  
Michael Koupparis
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Gas Flow ◽  
Raw Materials ◽  
Pharmaceutical Formulations ◽  
Reversed Phase ◽  
Hplc Method ◽  
Ich Guidelines ◽  
Development And Validation

In this work, ELS-Detector has been used for the development of an HPLC method for the determination of clarithromycin in pharmaceutical formulations (tablets and pediatric suspension). Isocratic reversed phase HPLC approach has been developed using a C-18 column (Waters Spherisorb 5 μm ODS2, 4.6x250 mm) and a mobile phase consisting of acetonitrile / aqueous trifluoroacetic acid as pairing reagent. Experimental parameters (temperature of heated drift tube, flow rate of mobile phase, gas flow rate, mobile phase composition) were optimized. Clarithromycin’ s stability was thoroughly examined in different solvent systems. Using the optimized conditions the working range was 5-100 μg/mL (upper limit can be increased considerably), with a detection limit of 4.5 μg/mL (6x10-6 M). The method was validated as per ICH guidelines. The retention time was 4.7 min. The method was successfully applied for the content assay of clarithromycin formulations.

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