Simultaneous RP-HPLC determination of sparfloxacin and dexamethasone in pharmaceutical formulations

Razzaq, Syed Naeem; Ashfaq, Muhammad; Mariam, Irfana; Khan, Islam Ullah; Razzaq, Syed Saleem

doi:10.1590/s1984-82502013000200012

Cited by 7 publications

(7 citation statements)

References 23 publications

(13 reference statements)

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“…The chemistry of separating analytes plays a role when selecting appropriate chromatographic conditions. Ciprofloxacin and dexamethasone drugs can be separated through reverse-phase stationary phases because of containing major non-polar groups as well as containing unsaturated π electrons as demonstrated in our previous studies [28,36]. Polar stationary phases like cyano, can also be used as groups like (-COOH, -OH or F etc.)…”

Section: -Results and Discussionmentioning

confidence: 96%

“…During initial experiments, dexamethasone peaks showed high tailing on C18, Phenyl-2, and Cyano columns but symmetrical/good peak on C8 [28,36]. However when same conditions were applied to ciprofloxacin using C8 column, tailed peak (tailing factor 1.99) was observed.…”

Section: Optimization Of Mobile Phase and Stationary Phasementioning

confidence: 96%

“…Reviewing the literature resulted in the occurrence of few methods for this FDC [22][23], however no stability indicating HPLC method was found for this FDC. We are involved recently to conduct research relating to method development of FDC of different drugs with varying chemical properties and many of these papers have been reported in the literature [24][25][26][27][28][29][30][31][32][33][34][35][36]. In order to fill this knowledge gap, it was attempted to develop and validate HPLC method with stability indicating properties for this FDC (ciprofloxacin and dexamethasone) not only in commercial formulations but also in human serum and urine.…”

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confidence: 99%

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Stability Indicating Rp-HPLC Method for Simultaneous Determination of Ciprofloxacin and Dexamethasone in Binary Combination

Razzaq

Ashfaq

Mariam³

et al. 2017

J. Chil. Chem. Soc.

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A simple and isocratic HPLC method with stability indicating nature was developed and then subsequently validated for simultaneous determination of ciprofloxacin and dexamethasone in pharmaceutical formulations, human serum and urine. Best chromatographic separations were attained within run time of 10 minutes using C8 as stationary phase and mixture of phosphate buffer and methanol (41:59 v/v) as mobile phase. The mobile phase was flowed at 1.5 mL min -1 with detection of both the analytes at 270 nm using photodiode array detector. Validation of the method was accomplished using specificity, linearity, accuracy, precision, robustness, LOD and LOQ. The method was found linear from 3-21 mg mL -1 for ciprofloxacin (r 2 ≥ 0.999) and 1-7 mg mL -1 for dexamethasone (r 2 ≥ 0.999). The %age recoveries of ciprofloxacin in spiked human urine and serum were ≥99% and ≥85% respectively, while for dexamethasone they were ≥97% in both matrices. The method proficiently separated the peaks of ciprofloxacin and dexamethasone from all types of interfering substances including degradation products/impurities with purity index ≥ 0.9998. The method thus was stability-indicating and can be employed for simultaneous analysis of ciprofloxacin and dexamethasone in complex matrices involving multiple components in the mixture. 1-INTRODUCTION Ciprofloxacin(1-cyclopropyl-6-fluoro-4-oxo-7-(piperazin-1-yl)-quinoline-3-carboxylic acid), a well-known antibiotic, is used to relieve bacterial infections of the eyes, corneal ulcers along with some common bacterial attacks. Dexamethasone (8S,9R,10S,11S,13S,14S,1 6R,17R)-9-Fluoro-11,17-dihydroxy-17-(2-hydroxyacetyl)-10, 13,16-trimethyl-,7,8,9,10,11,12,13,14,15,16,17-dodecahydro-3H-cyclopenta[a] phenanthren-3-one [ Figure 1] also the enforcement agencies in general to monitor the quality of the marketed products. 2-EXPERIMENTAL Chemicals and ReagentsCiprofloxacin (99.87%) and dexamethasone (99.96%) reference standards were received from Schazoo Zaka Laboratories (Lahore, Pakistan) and were used as such without further refinement. Commercial products (Zoxan D and Ciprodex) containing 3 mg mL -1 ciprofloxacin and 1 mg mL -1 dexamethasone were analyzed during the current research work. All the chemicals used were of either HPLC grade or highest grade available commercially and were used as such. Double distilled water, other liquids used in mobile phase and all the injecting solutions were subject to filtration employing 0.45 mm nylon filters (Millipore, USA). Equipment and Chromatographic ConditionsAll the chromatographic work was conducted on LC-20A system (Shimadzu, Japan) using PDA detector at 270 nm. Each time 20 mL volume of analytes were injected using the fixed loop and peak areas of ciprofloxacin and dexamethasone were integrated using system built software. For separation, Hypersil BDS C8 column (250 X 4.6 mm, 5 mm) was used at room temperature. Pre-mixed mobile phase was used which was prepared by mixing 59:41 v/v ratio of methanol and 0.018M phosphate buffer (pH 3.0) and was flowe...

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Section: -Results and Discussionmentioning

confidence: 96%

Section: Optimization Of Mobile Phase and Stationary Phasementioning

confidence: 96%

mentioning

confidence: 99%

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Stability Indicating Rp-HPLC Method for Simultaneous Determination of Ciprofloxacin and Dexamethasone in Binary Combination

Razzaq

Ashfaq

Mariam³

et al. 2017

J. Chil. Chem. Soc.

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“…Similarly, the estimation of dexamethasone has also been reported widely by HPLC (Iqbal et al, 2006;Huetos et al, 1999; gap, the present study was designed to optimize the chromatographic conditions in order to estimate them in different matrices (pharmaceutical formulations, human urine and serum). In the past few years, different FDC have already been reported by our research group after developing suitable analytical methods Khan et al, 2013;Razzaq et al, 2013;John et al, 2015a, b;Saleem et al, 2015).…”

Section: Introductionmentioning

confidence: 98%

Stability indicating RP-HPLC method for simultaneous determination of gatifloxacin and dexamethasone in binary combination

Razzaq

Ashfaq

Khan

et al. 2017

Braz. J. Pharm. Sci.

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In this study, conditions were optimized for development of a simple RP-HPLC method for simultaneous analysis of gatifloxacin and dexamethasone in different matrices like pharmaceuticals, human serum and urine. Good separation of gatifloxacin and dexamethasone from the induced degradation products was accomplished using C8 as stationary phase; 0.02 M phosphate buffer (pH 3. .999). Both the analyte peaks were completely separated from the peaks of induced degradation products as indicated by the peak purity index (≥0.9999 for both analytes). The optimized method is recommended to be used for concurrent analysis of gatifloxacin and dexamethasone in different matrices.

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“…Efforts were therefore made to develop a novel, fast and validated stability indicating HPLC procedure for determining simultaneously both the drugs in pharmaceutical dosage forms and human serum. Currently we are developing analytical methods for drugs in binary combinations [16][17][18][19][20][21][22][23][24] and this study is a continuation of the previous work as it contained two active ingredients in formulation.…”

Section: Introductionmentioning

confidence: 99%

Stability-indicating RP-HPLC method for simultaneous determination of methoxsalen and p-aminobenzoic acid in binary combination

John¹,

Azeem²,

Ashfaq³

et al. 2015

Bull. Chem. Soc. Eth.

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ABSTRACT. An accurate, simple and specific reverse phase LC procedure is established and validated for simultaneous estimation of methoxsalen and p-aminobenzoic acid in pharmaceutical formulated products and human serum. Chromatographic separation among methoxsalen, p-aminobenzoic acid and their degradation products have been achieved in less than 5 min with Hypersil-ODS column (250 mm x 4.6 mm, 5 µm), using acetonitrile and 1.28 mM phosphate buffer as mobile phase (60:40 v/v). Flow rate of the mobile phase was set as 1.5 mL min -1 and detection of all the analytes was carried out by diode-array detector at 254 nm. The developed method was validated according to ICH guidelines by performing its linearity, accuracy, precision, specificity, robustness and LOD/LOQ values. Response was linear and proportional to the concentrations (24-48 µg mL -1 ) for p-aminobenzoic acid and (9-18 µg mL -1 ) for methoxsalen. The LOD was 2.3 ng mL -1 for p-aminobenzoic acid and 6 ng mL -1 for methoxsalen whereas LOQ was 7.8 ng mL -1 for p-aminobenzoic acid and 20.4 ng mL -1 for methoxsalen. The developed method efficiently separated the principal peaks from degradation products and therefore can be applied successfully for concurrent analysis of methoxsalen and p-aminobenzoic acid in pharmaceutical dosage form, human serum and product stability studies.

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Simultaneous RP-HPLC determination of sparfloxacin and dexamethasone in pharmaceutical formulations

Cited by 7 publications

References 23 publications

Stability Indicating Rp-HPLC Method for Simultaneous Determination of Ciprofloxacin and Dexamethasone in Binary Combination

Stability Indicating Rp-HPLC Method for Simultaneous Determination of Ciprofloxacin and Dexamethasone in Binary Combination

Stability indicating RP-HPLC method for simultaneous determination of gatifloxacin and dexamethasone in binary combination

Stability-indicating RP-HPLC method for simultaneous determination of methoxsalen and p-aminobenzoic acid in binary combination

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