scholarly journals A Comparative Study of Newly Developed HPLC-DAD and UHPLC-UV Assays for the Determination of Posaconazole in Bulk Powder and Suspension Dosage Form

2014 ◽  
Vol 2014 ◽  
pp. 1-7 ◽  
Author(s):  
Dalia A. Hamdy ◽  
Tarek S. Belal
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Gradient Elution ◽  
Potassium Dihydrogen ◽  
Bulk Powder ◽  
Ich Guidelines ◽  
The Mean ◽  
Potassium Dihydrogen Orthophosphate ◽  
Dihydrogen Orthophosphate

Objective. To develop and compare HPLC-DAD and UHPLC-UV assays for the quantitation of posaconazole in bulk powder and suspension dosage form.Methods. Posaconazole linearity range was 5–50 μg/mL for both assays. For HPLC-DAD assay, samples were injected through Zorbax SB-C18 (4.6 × 250 mm, 5 μm) column. The gradient elution composed of the mobile phase acetonitrile: 15 mM potassium dihydrogen orthophosphate (30 : 70 to 80 : 20, linear over 7 minutes) pumped at 1.5 mL/min. For UHPLC-UV assay, samples were injected through Kinetex-C18 (2.1 × 50 mm, 1.3 μm) column. The mobile phase composed of acetonitrile: 15 mM potassium dihydrogen orthophosphate (45 : 55) pumped isocratically at 0.4 mL/min. Detection wavelength was 262 nm in both methods.Results. The run time was 11 and 3 minutes for HPLC-DAD and UHPLC-UV assays, respectively. Both assays were linear (r2>0.999) with CV% and % error of the mean <3%. Limits of detection and quantitation were 0.82 and 2.73 μg/mL for HPLC-DAD and 1.04 and 3.16 μg/mL for UHPLC-UV, respectively. The methods quantitated PSZ in suspension dosage form with no observable interferences.Conclusions. Both assays were proven sensitive and selective according to ICH guidelines. UHPLC-UV assay exhibited some economic and chromatographic separation superiority.

scholarly journals DETERMINATION OF CHROMATOGRAPHIC ASSAY AND VALIDATION OF OFLOXACIN IN BULK AND PHARMACEUTICAL DOSAGE FORM

2018 ◽  
Vol 11 ◽  
Author(s):  
Sumithra M
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Assay Method ◽  
Reverse Phase ◽  
Pharmaceutical Dosage Form ◽  
Ich Guidelines ◽  
Validation Parameters ◽  
The Mean

Objective: The objective of the study is simple, sensitive; eco-friendly reverse phase chromatographic method has been developed and validated for the quantitative determination of ofloxacin in bulk and marketed formulation. Method: The developed method was done using Hypersil silica C18 (250 mm × 4.6 mm, 5 μ particle size) as column and the mobile phase is containing water and methanol in the ratio of (10:90) vol/vol. The mobile phase pass at 1 ml/min flow rate and the eluted solution is measured at 270 nm using a PDA detector. Results: The assay method is linear from the concentration range of 5–30 μg/ml. The corelation coefficient is 0.9998. The mean percentage recovery for the developed method is found to be in the range of 98.4–100.6%. The developed method complies robustness studies. Conclusion: The validation of the developed method was done by as per the ICH guidelines. It obeys the linearity, accuracy, precision, and robustness studies. Validation parameters are within the limitations. The results of the developed process indicated the reverse phase chromatographic method is simple, accurate as well as precise, rapid and eco-friendly method for routine analysis of ofloxacin in bulk and its pharmaceutical dosage form.

A Versatile Stability-indicating Liquid Chromatographic Method for the Simultaneous Determination of Atenolol, Hydrochlorothiazide and Chlorthalidone

2020 ◽  
Vol 16 (8) ◽  
pp. 1037-1051
Author(s):  
Ehab Farouk Elkady ◽  
Marwa Ahmed Fouad ◽  
Abdulgabar A. Ezzy Faquih
Keyword(s):  
Quality Control ◽  
Chromatographic Method ◽  
Degradation Products ◽  
Pharmaceutical Dosage Forms ◽  
Potassium Dihydrogen ◽  
Ich Guidelines ◽  
Liquid Chromatographic Method ◽  
Liquid Chromatographic ◽  
Potassium Dihydrogen Orthophosphate

Background: Atenolol is a selective beta 1 blocker that can be used alone or in combination with hydrochlorothiazide or with chlorthalidone for the treatment of hypertension and prevention from a heart attack. Objective: The main target of this work was to improve modern, easy, accurate and selective liquid chromatographic method (RP-HPLC) for the determination of these drugs in the presence of their degradation products. These methods can be used as analytical gadgets in quality control laboratories for a routine examination. Methods: In this method, the separation was accomplished through an Inertsil® ODS-3V C18 column (250 mm x 4.6 mm, 5 μm), the mobile phase used was 25 mM aqueous potassium dihydrogen orthophosphate solution adjusted to pH 6.8 by using 0.1M sodium hydroxide and acetonitrile (77 : 23, v/v), the flow rate used was 1 ml/min and detection was achieved at 235 nm using UV. Results: All peaks were sharp and well separated, the retention times were atenolol degradation (ATN Deg.) 2.311 min, atenolol (ATN) 2.580 min, hydrochlorothiazide degradation (HCT Deg.) 5.890 min, hydrochlorothiazide (HCT) 7.016 min, chlorthalidone degradation CTD Deg 8.018 min and chlorthalidone (CTD) 14.972 min. Linearity was obtained and the range of concentrations was 20- 160 μg/ml for atenolol, 10-80 μg/ml for hydrochlorothiazide and 10-80 μg/ml for chlorthalidone. According to ICH guidelines, method validation was accomplished, these methods include linearity, accuracy, selectivity, precision and robustness. Conclusion: The optimized method demonstrated to be specific, robust and accurate for the quality control of the cited drugs in pharmaceutical dosage forms.

Structural Elucidation of Potential Impurities in Azilsartan Bulk Drug by HPLC

2014 ◽  
Vol 97 (6) ◽  
pp. 1552-1562
Author(s):  
Wentao Zhou ◽  
Yuxia Zhou ◽  
Lili Sun ◽  
Qiaogen Zou ◽  
Ping Wei ◽  
...  
Keyword(s):  
Phosphoric Acid ◽  
Correlation Coefficient ◽  
Chromatographic Method ◽  
Hplc Method ◽  
Potassium Dihydrogen ◽  
The Mean ◽  
Bulk Drug ◽  
Potassium Dihydrogen Orthophosphate ◽  
Gradient Mode ◽  
Dihydrogen Orthophosphate

Abstract During the synthesis of Azilsartan (AZS), it was speculated that 15 potential impurities would arise. This study investigated the possible mechanism for the formation of 14 of them, and their structures were characterized and confirmed by IR, NMR, and MS techniques. In addition, an efficient chromatographic method was developed to separate and quantify these impurities, using an Inertsil ODS-3 column (250 × 4.6 mm, 5 μm) in gradient mode with a mixture of acetonitrile and the potassium dihydrogen orthophosphate buffer (10 mM, pH adjusted to 3.0 with phosphoric acid). The HPLC method was validated for specificity, precision, accuracy, and sensitivity. LOQ of impurities were in the range of 1.04–2.20 ng. Correlation coefficient values of linearity were &gt;0.9996 for AZS and its impurities. The mean recoveries of all impurities in AZS were between 93.0 and 109.7%. Thus, the validated HPLC method is suitable for the separation and quantification of all potential impurities in AZS.

Stability-Indicating Methods for the Determination of Candesartan Cilexetil in Bulk Drug and Pharmaceutical Formulations

2013 ◽  
Vol 96 (3) ◽  
pp. 580-586 ◽  
Author(s):  
Yousry M Issa ◽  
Emad M Hussien ◽  
Magda M Ibrahim ◽  
Fatma M Abdel-Gawad ◽  
Saadia Barakat
Keyword(s):  
Mobile Phase ◽  
Candesartan Cilexetil ◽  
Degradation Products ◽  
Pharmaceutical Formulations ◽  
Stability Indicating ◽  
Bulk Powder ◽  
System Suitability ◽  
The Mean ◽  
Bulk Drug

Abstract Two stability-indicating methods were developed for the determination of candesartan cilexetil in the presence of its degradation products. The first method uses isocratic RP-HPLC with an Agilent C18 column. The mobile phase was phosphate buffer (pH = 2.8 ± 0.1)–acetonitrile (60 + 40, v/v). The flow rate was 2.0 mL/min, and the UV detection was at 254 nm. The second method depends on TLC-densitometric measurements of drug spots at 254 nm. The separation was carried out on silica gel 60 F254 plates using ethyl acetate–methanol–toluene– ammonia 33% (40 + 25 + 20 + 2, v/v/v/v) mobile phase. The methods were validated according to U.S. Pharmacopeia guidelines, and the acceptance criteria for accuracy, precision, linearity, specificity, robustness, LOD, LOQ, and system suitability were met in all cases. Linear ranges of the methods were 10.0–200.0 μg/mL and 1.0–9.0 μg/spot for HPLC and TLC, respectively. The proposed methods were successfully applied to the drug in bulk powder, in laboratory-prepared mixtures with its degradation products, and in commercially available tablets. The results were compared statistically at the 95% confidence level with each other. There were no significant differences between the mean recovery and precision of the two methods.

scholarly journals Development and validation of novel RP-UPLC method for estimation of atropine sulphate in pharmaceutical dosage form

2013 ◽  
Vol 19 (3) ◽  
pp. 333-337 ◽  
Author(s):  
A.C. Arvadiya ◽  
P.P. Dahivelker
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Limit Of Detection ◽  
Atropine Sulphate ◽  
Limit Of Quantification ◽  
Pharmaceutical Dosage Form ◽  
Column Temperature ◽  
Ich Guidelines ◽  
Development And Validation

A simple, precise, accurate, sensitive and repeatable RP-UPLC method was developed for quantitative determination of atropine sulphate in pharmaceutical dosage form. The method was developed by using C18 column Hiber HR Purospher Star (100mm?2.1mm id, 2?m particle size) as stationary phase with Phosphate Buffer: Acetonitrile (87:13, %v/v) as a mobile phase, pH was adjusted to 3.5 by ortho-phosphoric acid at a flow rate of 0.5 mL/min and column temperature maintained at 30?C. Quantification of eluted compound was achieved with PDA detector at 210 nm. Atropine sulphate followed linearity in concentration range of 2.5-17.5 ?g/mL with r2=0.9998 (n=6). Limit of detection (LOD) and limit of quantification (LOQ) values were 0.0033 and 0.0102 ?g/mL for atropine sulphate. The validation study is carried out as per International Conference on Harmonization (ICH) guidelines. This method was successfully applied for estimation of atropine sulphate in pharmaceutical formulation.

scholarly journals Stability indicating RP-HPLC method for the estimation of flucloxacillin sodium in a tablet dosage form

2020 ◽  
Vol 1 (4) ◽  
pp. 95-100
Author(s):  
Sonalika Patro ◽  
S. Harshith Kumar ◽  
M. Barath kumar ◽  
E. Masthaniah ◽  
K. Sairam ◽  
...  
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Theoretical Plate ◽  
Hplc Method ◽  
Rp Hplc ◽  
Ich Guidelines ◽  
System Suitability ◽  
Precision Study ◽  
Tablet Dosage

A Simple, accurate and precise method was developed and validated for the determination of flucloxacillin sodium in its tablet dosage form. The separation was eluted on xterra c18 column (4.6x150mm, 5micron) using a mixture of octane buffer and methanol as mobile phase in a ratio of (30:70) which was pumped through column at a flow rate of  1ml/min. Optimised wavelength for flucloxacillin was 237nm, the retention time was 2.305minutes and the percentage purity was found to be 98.14%. System suitability parameters such as theoretical plate and tailing factor for flucloxacillin sodium was found to be 2991.64 and 1.90 respectively, the proposed method was validated as per ICH guidelines (ICH, Q2 AND (R1)) the method was found to be linear at the concentration range of 20-100µg/ml and the correlation coefficient (r2) value was found to be 0.9994 percentage RSD for precision was 0.9% and percentage RSD for ruggedness was 0.5%. The precision study was precise, robust and repeatable. The LOD and LOQ values are 2.98 and 9.98 respectively. Hence the suggested RP-HPLC method can be used for routine analysis for flucloxacillin sodium in tablet dosage form.

scholarly journals Simultaneous UV Spectrophotometric Estimation of Amlodipine and Chlorthalidone in Bulk and Combined Tablet Dosage Form

2019 ◽  
pp. 468-472
Author(s):  
Sunil More ◽  
Ashpak Tamboli ◽  
Snehal Patil ◽  
Amol Vhanmane
Keyword(s):  
Spectrophotometric Method ◽  
Mobile Phase ◽  
Dosage Form ◽  
Spectroscopic Method ◽  
Simultaneous Equation ◽  
Ich Guidelines ◽  
Combined Estimation ◽  
Tablet Dosage ◽  
Different Levels

There is not a single analytical methods appeared in the literature for combined estimation of Amlodipine and Chlorthalidone in tablets dosage form. Attempts were made to develop a simple, precise and accurate Simultaneous UV spectroscopic method of Amlodipine and Chlorthalidone in bulk and Amlodac CH tablet dosage form by using simultaneous equation method. UV spectrophotometric method was developed and validated as per ICH guidelines using methanol as mobile phase. Amlodipine and Chlorthalidone individually follows the Beer-Lamberts law over concentration range 2.5-12.5μg/ml and 6.25-31.5μg/ml, Regression of coefficient was found to be r2=0.999 and r2=0.999 respectively. The percentage recovery was found in the range of 98% to 102% at three different levels. The proposed method was successfully applied for the determination of Amlodipine and Chlorthalidone in tablets dosage form as per ICH guidelines the result of the analysis were validated statistically and were found to be satisfactory.

APPLICATION OF HPTLC AND RP-HPLC METHODS FOR SIMULTANEOUS ESTIMATION OF OFLOXACIN AND PREDNISOLONE ACETATE IN OPHTHALMIC DOSAGE FORM

INDIAN DRUGS ◽  
2015 ◽  
Vol 52 (05) ◽  
pp. 17-26
Author(s):  
M. L Chavhan ◽  
◽  
A. S Patil ◽  
S. J Surana ◽  
A. A. Shirkhedkar
Keyword(s):  
Mobile Phase ◽  
Dosage Form ◽  
Internal Standard ◽  
Prednisolone Acetate ◽  
Simultaneous Estimation ◽  
Hplc Separation ◽  
Potassium Dihydrogen ◽  
Rp Hplc ◽  
Ophthalmic Formulation

Two simple, rapid, precise, accurate and robust (HPTLC and RP-HPLC) methods have been established for simultaneous determination of ofloxacin and prednisolone acetate in its combined ophthalmic formulation. HPTLC separation of two drugs was accomplished on a HPTLC aluminum-backed layer of silica gel 60 F254 using n-butanol: methanol: ammonia (60:10:30% V/V/V) as a mobile phase. The densitometric scanning was performed at 275 nm which showed Rf 0.43 for ofloxacin and 0.78 for prednisolone acetate, respectively. RP-HPLC separation of the two drugs was achieved on LC-GC Qualisil BDS C-18 column using mobile phase methanol: acetonitrile: 0.02 M potassium dihydrogen ortho-phosphate anhydrous (50:15:35% V/V/V), pH adjusted to 4.5 with triethylamine. Detection of both drugs was done at 275 nm. Aspirin was used as an internal standard (IS). The retention time for ofloxacin, prednisolone acetate and aspirin (IS), was found to be 4.36 min. and 6.60 min and 3.55 min, respectively. The proposed methods were successfully applied for the determination of both drugs in bulk and in combined ophthalmic formulation. Assay of both these methods were compared using student t-test.

VALIDATED HPTLC METHOD FOR SIMULTANEOUS DETERMINATION OF OLMESARTAN MEDOXIMIL AND METOPROLOL SUCCINATE IN TABLET DOSAGE FORM

INDIAN DRUGS ◽  
2012 ◽  
Vol 49 (10) ◽  
pp. 13-17
Author(s):  
V. V Kunjir ◽  
◽  
S. B. Jadhav ◽  
A. J Purkar ◽  
P. D. Chaudhari
Keyword(s):  
Simultaneous Determination ◽  
Mobile Phase ◽  
High Performance ◽  
Dosage Form ◽  
Chromatographic Method ◽  
Metoprolol Succinate ◽  
Ich Guidelines ◽  
Tablet Dosage ◽  
Hptlc Method

A high performance thin layer chromatographic method has been developed for the simultaneous determination of olmesartan medoximil and metoprolol succinate from tablet dosage form. The mobile phase consisting of water-methanol-ammonium sulphate (4.5:4.5:1.5 v/v/v) and wavelength of detection 233 nm was used. The developed method was validated as per ICH guidelines.

scholarly journals A Validated RP-HPLC Method for Simultaneous Estimation of Atenolol and Indapamide in Pharmaceutical Formulations

2011 ◽  
Vol 8 (3) ◽  
pp. 1238-1245 ◽  
Author(s):  
G. Tulja Rani ◽  
D. Gowri Sankar ◽  
P. Kadgapathi ◽  
B. Satyanarayana
Keyword(s):  
Particle Size ◽  
Mobile Phase ◽  
Dosage Form ◽  
Orthophosphoric Acid ◽  
Pharmaceutical Formulations ◽  
Hplc Method ◽  
Simultaneous Estimation ◽  
Rp Hplc ◽  
Ich Guidelines

A simple, fast, precise, selective and accurate RP-HPLC method was developed and validated for the simultaneous determination of atenolol and indapamide from bulk and formulations. Chromatographic separation was achieved isocratically on a Waters C18 column (250×4.6 mm, 5 µ particle size) using a mobile phase, methanol and water (adjusted to pH 2.7 with 1% orthophosphoric acid) in the ratio of 80:20. The flow rate was 1 mL/min and effluent was detected at 230 nm. The retention time of atenolol and indapamide were 1.766 min and 3.407 min. respectively. Linearity was observed in the concentration range of 12.5-150 µg/mL for atenolol and 0.625-7.5 µg/mL for indapamide. Percent recoveries obtained for both the drugs were 99.74-100.06% and 98.65-99.98% respectively. The method was validated according to the ICH guidelines with respect to specificity, linearity, accuracy, precision and robustness. The method developed can be used for the routine analysis of atenolol and indapamide from their combined dosage form.

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