A study of the separation of Mo(VI) and W(VI) by reversed phase HPLC

1989 ◽  
Vol 54 (8) ◽  
pp. 2133-2140 ◽  
Author(s):  
Milan Vrchlabský ◽  
Naděžda Pollaková ◽  
Aleš Hrdlička
Keyword(s):  
Flow Rate ◽  
Phosphate Buffer ◽  
Stream Flow ◽  
Mobile Phase ◽  
Reversed Phase ◽  
Reversed Phase Hplc ◽  
Hplc Separation ◽  
Rp Hplc

The RP HPLC separation of Mo(VI) and W(VI) in the form of their oxoanions or anionic chelates with 2,3-dihydroxynaphthalene (DHN) was studied using a 100 x 4 mm i.d. column packed with Silasorb C18 (10μm). The two elements were separated with a resolution of Rij = 1.8 in 10 min after injection of the DHN-derivatized anions into the stream (flow rate 1 ml min-1) of the mobile phase containing phosphate buffer (50 mmol l-1), DHN (0.5 mmol l-1) and tetrabutylammonium cations (1 mmol l-1) in 60% (v/v) methanol at pH 7.

SIMULTANEOUS ESTIMATION OF CURCUMIN AND GEFITINIB IN BULK AND TISSUE SAMPLES (PLASMA AND BRAIN HOMOGENATE) BY RP-HPLC: APPLICATION TO A DISTRIBUTION STUDY

INDIAN DRUGS ◽  
2019 ◽  
Vol 56 (07) ◽  
pp. 59-68
Author(s):  
H Mahajan ◽  
S Savale ◽  
P Nerkar ◽  
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
Internal Standard ◽  
Brain Homogenate ◽  
Reversed Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Bulk Analysis ◽  
Experimental Conditions ◽  
Rp Hplc

The present study was aimed at developing a Reversed-Phase High-Performance Liquid Chromatography (RP-HPLC) method for simultaneous determination of curcumin (CRM) and gefitinib (GFT) in bulk, plasma and brain homogenate. hydrochlorothiazide was used as an internal standard (IS). A new simple, rapid, selective, precise and accurate RP-HPLC method has been developed. The separation was achieved by using C-18 column (Qualisil BDS C18, 250 mm x 4.6 mm I.D.) coupled with a guard column of silica, mobile phase consisted of acetonitrile: water with 0.1% formic acid (30:70 v/v). The flow rate was 0.2 ml/min and the drug was detected using PDA detector at the wavelength of 242 nm. The experimental conditions, including the diluting solvent, mobile phase composition, column saturation and flow rate, were optimised to provide high-resolution and reproducible peaks. The method was developed and tested for linearity range of 10-60 μg/mL for bulk analysis and 200-800 ng/mL for plasma and brain homogenate. The developed method was validated as per ICH guidelines, in terms of linearity, application of the proposed method to bulk sample, recovery, precision, repeatability, ruggedness, sensitivity (LOD and LOQ) and robustness and stability study (short and long-term stabilities, freeze/thaw stability, post-preparative). The low value of % RSD showed that the method was precise within the acceptance limit of 2%. The developed method was successfully applied for the analysis of the drug in bulk as well as various marketed formulation and drug in plasma and brain distribution studies.

scholarly journals Application of a reversed-phase HPLC method for quantitative p-coumaric acid analysis in wine

OENO One ◽  
2010 ◽  
Vol 44 (2) ◽  
pp. 117
Author(s):  
Dominique Salameh ◽  
Cédric Brandam ◽  
Toufic Rizk ◽  
Roger Lteif ◽  
Pierre Strehaiano
Keyword(s):  
Mobile Phase ◽  
Chromatographic Method ◽  
Red Wine ◽  
Reversed Phase ◽  
Hplc Method ◽  
Coumaric Acid ◽  
Reversed Phase Hplc ◽  
Mobile Phase Composition ◽  
Rp Hplc ◽  
Synthetic Media

<p style="text-align: justify;"><strong>Aims</strong>: This paper presents a rapid chromatographic method to monitor the concentration of <em>p</em>-coumaric acid in wine and in bioconversion studies.</p><p style="text-align: justify;"><strong>Methods and results</strong>: RP-HPLC method was validated in synthetic wine medium and in natural red wine. Mobile phase composition was water 77%, acetonitrile 23%. Formic acid was added to control pH at 3.5. The flow was 0.7 mL/min and the temperature 30 °C. The detection was done using UV at 305 nm. The linearity range was validated between 0.5 and 15 mg/L. The resolution was respectively 5.35 and 2.99. The detection and quantification limits were 0.01 mg/L and 0.04 mg/L. This method was used to study <em>p</em>-coumaric acid bioconversion into 4-ethylphenol and 4-vinylphenol, and to study this acid adsorption in enological conditions.</p><p style="text-align: justify;"><strong>Conclusions</strong>: This paper presented a simple HPLC method to monitor the concentration of <em>p</em>-coumaric acid in synthetic media and natural wine. It was used to study the <em>p</em>-coumaric acid bioconversion rates and mechanism.</p><p style="text-align: justify;"><strong>Significance and impact of the study</strong>: This method is useful to monitor <em>p</em>-coumaric acid concentration, which helps to predict amounts of 4-ethylphenol or 4-vinylphenol that can be produced in wine. This method can be helpful to control undesirable phenolic flavors potential in wine.</p>

TLC-Densitometric and RP-HPLC Methods for Simultaneous Determination of Dexamethasone and Chlorpheniramine Maleate in the Presence of Methylparaben and Propylparaben

2017 ◽  
Vol 100 (1) ◽  
pp. 51-58
Author(s):  
Nehal F Farid ◽  
Ibrahim A Naguib ◽  
Radwa S Moatamed ◽  
Mohamed R El Ghobashy
Keyword(s):  
Particle Size ◽  
Quantitative Determination ◽  
Mobile Phase ◽  
Ammonium Acetate ◽  
Reversed Phase ◽  
Reversed Phase Hplc ◽  
Chlorpheniramine Maleate ◽  
Ammonium Acetate Buffer ◽  
Rp Hplc

Abstract Validated simple, sensitive, and highly selective methods are applied for the quantitative determination ofdexamethasone and chlorpheniramine maleate in the presence of their reported preservatives (methylparaben and propylparaben), whether in pure forms or in pharmaceutical formulation. TLC is the first method, in which dexamethasone, chlorpheniramine maleate, methylparaben, and propylparaben are separated on silica gel TLC F254 plates using hexane–acetone–ammonia (5.5 + 4.5 + 0.5, v/v/v) as the developing phase. Separated bands are scanned at 254 nm over a concentration range of 0.1–1.7 and 0.4–2.8 μg/band, with mean ± SD recoveries of 99.12 ± 0.964 and 100.14 ± 0.962%, for dexamethasone and chlorpheniramine maleate, respectively. Reversed-phase HPLC is the second method, in which a mixture of dexamethasone and chlorpheniramine maleate, methylparaben, and propylparaben is separated on a reversed-phase silica C18 (5 μm particle size, 250 mm, 4.6 mm id) column using 0.1 M ammonium acetate buffer–acetonitrile (60 + 40, v/v, pH 3) as the mobile phase. The drugs were detected at 220 nm over a concentration range of 5–50 μg/mL, 2–90 μg/mL, 4–100 μg/mL, and 7–50μg/mL, with mean ± SD recoveries of 100.85 ± 0.905, 99.67 ± 1.281, 100.20 ± 0.906, and 99.81 ± 0.954%, for dexamethasone, chlorpheniramine maleate, methylparaben paraben, and propylparaben, respectively. The advantages of the suggested methods over previously reported methods are the ability to detect lower concentrations of the main drugs and to show better resolution of interfering preservatives; hence, these methods could be more reliable for routine QC analyses.

scholarly journals ANALYTICAL QUALITY-BY-DESIGN (AQBD) APPROACH FOR THE DEVELOPMENT AND VALIDATION OF RP-HPLC METHOD FOR THE ESTIMATION OF LAMOTRIGINE IN BULK AND TABLET FORMULATION

2021 ◽  
Vol 10 (5) ◽  
pp. 3591-3596
Author(s):  
Manisha P. Puranik
Keyword(s):  
Flow Rate ◽  
Mobile Phase ◽  
High Performance ◽  
Quality By Design ◽  
Active Pharmaceutical Ingredient ◽  
Reversed Phase ◽  
Hplc Method ◽  
Analytical Technique ◽  
Rp Hplc ◽  
Ich Guideline

The current analytical exploration illustrated developing a reversed-phase high-performance liquid chromatography (RP-HPLC) technique and consequent substantiation for analyzing lamotrigine (LAM) active pharmaceutical ingredient (API) using a Quality-by-design (QbD) approach (Central Composite Design), in bulk product as well as in the tablet formulations. In this experiment, based on systematic scouting, four key components (viz., mobile phase, column, flow-rate, and wavelength) were studied by the RP-HPLC method. 13 experimental runs were done with acetonitrile (ACN) (40-60% v/v) having flow-rate in the range 0.8 mL/min to 1.2 mL/min. The proposed analytical method was thoroughly corroborated in terms of ruggedness linearity, robustness, accuracy, and precision in accordance with ICH guideline Q2A and ICH guideline Q2B. Under the optimum chromatographic environment; Intersil C8 column of 250 mm length, 4.6 mm (i.d.); 20 μL injection volume; and mobile phase ACN: Methanol (60:40 v/v), a retention time of 2.542 min was noticed at 220 nm detection wavelength. The method was found to be extremely reproducible, accurate, linear, precise, robust, and economically adequate to execute the estimation. The intended analytical technique was thoroughly assessed through statistical tools and could be an imperative concern for the habitual scrutiny of LAM in bulk products and its formulation.

SIMULTANEOUS DETERMINATION OF PARACETAMOL, ACECLOFENAC AND TRAMADOL HYDROCHLORIDE IN PHARMACEUTICAL DOSAGE FORM BY RP-HPLC METHOD

INDIAN DRUGS ◽  
2021 ◽  
Vol 58 (01) ◽  
pp. 35-40
Author(s):  
Rajesh Sharma ◽  
◽  
Mukesh C. Sharma ◽  
Gaurav Vijaywargiya
Keyword(s):  
Flow Rate ◽  
Chromatographic Separation ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Dosage Form ◽  
Hplc Method ◽  
Tramadol Hydrochloride ◽  
Pharmaceutical Dosage Form ◽  
Rp Hplc

Chromatographic separation of paracetamol, aceclofenac and tramadol hydrochloride was performed on a Chromatopak C-18 column (25 cm x 4.6mm i.d. x 5µm) as stationary phase with a mobile phase composed of phosphate buffer pH 7.0: acetonitrile (65:35 V/V), pH 7.0 (adjusted with triethylamine) at flow rate of 1mL/min. Detection was carried out at 265 nm. The retention times of paracetamol, aceclofenac and Tramadol hydrochloride were found to be 2.7, 4.5 and 6.0 min, respectively. The proposed method was validated for linearity, accuracy, precision, LOD and LOQ. The method was found to be accurate, precise, specific, robust, and linear for the determination of paracetamol, aceclofenac and tramadol hydrochloride in pharmaceutical dosage form.

scholarly journals Experimental Design Approach to Optimize HPLC Separation of Active Ingredients, Preservatives, and Colorants in Syrup Formulation

2019 ◽  
Vol 102 (5) ◽  
pp. 1523-1529
Author(s):  
Şule Dinç-Zor ◽  
Bürge Aşçi ◽  
Özlem Aksu Dönmez ◽  
Özge Hacimustafa
Keyword(s):  
Experimental Design ◽  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Pharmaceutical Products ◽  
Hplc Method ◽  
Optimum Conditions ◽  
Hplc Separation ◽  
Sunset Yellow ◽  
Second Gradient

Abstract Background: Preservatives and colorants in pharmaceutical products may be highly toxic, especially for sensitive individuals, when they are used in excessive amounts. In this context, sensitive and non-labor-intensive analytical methods with short analysis time for simultaneous quantification of these additive substances in drugs can meet all requirements in quality control laboratories. Objective: The aim of the study was to develop a simultaneous HPLC method for the analysis of pseudoephedrine HCl and guaifenesin, along with preservatives, methyl paraben and propyl paraben, and colorants, ponceau 4R and sunset yellow, in a syrup sample. Methods: Optimum conditions of HPLC separation were determined by Box-Behnken experimental design. Four independent variables of the separation were pH (6.0, 6.5, and 7.0) and flow rate of the mobile phase (2.0, 2.2, and 2.4 mL/min) and mobile phase ratios for the first and second gradient elutions (75, 80, and 85% for Gradient 1 and 50, 55, and 60% for Gradient 2 in terms of phosphate buffer percent, respectively). Results: The optimum conditions were found to be pH, 6.3; flow rate, 2.4 mL/min; and mobile phase ratios (phosphate buffer-acetonitrile) for Gradient 1 and 2, 85+15 (v/v) and 60+40 (v/v), respectively. Conclusions: Simultaneous analysis of all compounds was achieved by using this HPLC method with a short run time below 10 min. Highlights: This simple, rapid, and validated method is convenient and applicable for routine analysis of pharmaceutical products having similar composition without the need for any extraction step.

scholarly journals A Validated RP – HPLC Method for Simultaneous Estimation of Cefixime and Cloxacillin in Tablets

2008 ◽  
Vol 5 (3) ◽  
pp. 648-651 ◽  
Author(s):  
G. Rathinavel ◽  
P. B. Mukherjee ◽  
J. Valarmathy ◽  
L. Samueljoshua ◽  
M. Ganesh ◽  
...  
Keyword(s):  
Flow Rate ◽  
Retention Time ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc

This paper presents a RP-HPLC method for the simultaneous estimation of cefixime and cloxacillin in tablets. The process was carried out on C18column (5 μm, 25 cm × 4.6 mm, i.d) using phosphate buffer (pH 5.0), acetonitrile and methanol in the ratio 80:17:3 respectively as a mobile phase at a flow rate of 2mL/min. Wavelength was fixed at 225 nm. The retention time of cefixime and cloxacillin was found to be 5.657 and 6.200 min, respectively. The developed method is rapid and sensitive and it can be used for estimation of combination of these drugs in tablets.

scholarly journals Development and Validation of RP-HPLC Method for the Determination of Adefovir Dipivoxil in Bulk and in Pharmaceutical Formulation

2009 ◽  
Vol 6 (2) ◽  
pp. 469-474 ◽  
Author(s):  
Zaheer Ahmed ◽  
B. Gopinath ◽  
A. Sathish Kumar Shetty ◽  
B. K. Sridhar
Keyword(s):  
Flow Rate ◽  
Phosphate Buffer ◽  
Mobile Phase ◽  
Adefovir Dipivoxil ◽  
Hplc Method ◽  
Pharmaceutical Formulation ◽  
Rp Hplc ◽  
System Suitability ◽  
Development And Validation

A rapid and sensitive RP-HPLC method with UV detection (262 nm) for routine analysis of adefovir dipivoxil in bulk and in pharmaceutical formulation was developed. Chromatography was performed with mobile phase containing a mixture of acetonitrile and phosphate buffer (50:50, v/v) with flow rate 1.0 mL min-l. In the range of 5.0-100 µg/mL, the linearity of adefovir dipivoxil shows a correlation co-efficient of 0.9999. The proposed method was validated by determining sensitivity accuracy, precision, robustness stability, specificity, selectivity and system suitability parameters.

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