Dannana Gowri Sankar

Spectrophotometric Determination of Gemifloxacin Mesylate in Pharmaceutical Formulations Through Ion-Pair Complex Formation

Four simple and sensitive ion-pairing spectrophotometric methods have been described for the assay of gemifloxacin mesylate (GFX) either in pure form or in pharmaceutical formulations. The developed methods involve formation of colored chloroform extractable ion-pair complexes of the drug with safranin O (SFN O) and methylene blue (MB) in basic medium; Napthol blue 12BR (NB 12BR) and azocaramine G (AG) in acidic medium. The extracted complexes showed absorbance maxima at 525, 650, 620 and 540 nm for SFN O, MB, NB 12BR and AG, respectively.Beers law is obeyed in the concentration ranges 3-15, 4-20, 2-10 and 2-10 μg/mL with molar absorptivity of 2.81 × 104, 2.20 x 104, 4.02 × 104 and 4.15 × 104 L mole−1 cm−1 and relative standard deviation of 0.077, 0.104, 0.080 and 0.103% for SFN O, MB, NB 12BR and AG, respectively. These methods have been successfully applied for the assay of drug in pharmaceutical formulations. No interference was observed from common pharmaceutical adjuvants. Results of analysis were validated statistically and through recovery studies.

Utility of σ and π-Acceptors for the Spectrophotometric Determination of Gemifloxacin Mesylate in Pharmaceutical Formulations

In this study, four simple, fast, accurate and sensitive spectrophotometric methods have been developed for the determination of gemifloxacin mesylate in pharmaceutical formulations. The methods are based on the charge transfer complexation reaction of the drug as n-electron donor with sigma (σ)-acceptor iodine, and the pi (π)-acceptors 2, 3-dichloro-5, 6-dicyano-p-benzoquinone (DDQ)-7,7,8,8-tetra cyanoquinodimethane (TCNQ) and tetracyanoethylene (TCNE). The obtained charge transfer complexes were measured at 290nm for iodine (in 1, 2-dichloro ethane), at 470, 840 and 420 nm for DDQ, TCNQ and TCNE (in acetonitrile), respectively. Optimization of different experimental conditions is described. Beers law is obeyed in the concentration range of 6-30, 2-10, 2.5-12.5 and 1-5 μg mL−1 for iodine, DDQ, TCNQ and TCNE methods, respectively. The proposed methods were applied successfully to the determination of GFX in pharmaceutical formulations with good accuracy and precision.

Extractive Spectrophotometric Methods for the Determination of Rosuvastatin Calcium in Pure Form and in Pharmaceutical Formulations by Using Safranin O and Methylene blue

Two simple extractive Spectrophotometric methods are described for the determination of rosuvastatin calcium (RST) in pure form and in pharmaceutical formulations. These methods are based on the formation of ion association complexes of the RST with basic dyes safranin O (Method A) and methylene blue (Method B) in basic buffer of pH 9.8 followed by their extraction in chloroform. The absorbance of the chloroform layer for each method was measured at its appropriate λmax against the reagent blank. These methods have been statistically evaluated and are found to be precise and accurate.

Simple Spectrophotometric Determination of Torsemide in Bulk Drug and in Formulations

A simple and cost effective spectrophotometric method is described for the determination of torsemide in pure form and in pharmaceutical formulations. The method is based on the formation of blue colored chromogen when the drug reacts with Folin-Ciocalteu (F-C) reagent in alkaline medium. The colored species has an absorption maximum at 760 nm and obeys beers law in the concentration range 30 – 150 ug mL−1. The absorbance was found to increase linearly with increasing concentration of TSM, which is corroborated by the calculated correlation coefficient value of 0.9999 (n=8). The apparent molar absorptivity and sandell sensitivity were 1.896×103 L mol−1 cm−1 and 0.183 μg cm−2, respectively. The slope and intercept of the equation of the regression line are 5.4x10−3 and 1.00×10−4 respectively. The limit of detection was 0.94.The optimum experimental parameters for the reaction have been studied. The validity of the described procedure was assessed. Statistical analysis of the results has been carried out revealing high accuracy and good precision. The proposed method was successfully applied to the determination of TSM in pharmaceutical formulations.

Adaptation of Color Reactions for Spectrophotometric Determination of Pitavastatin Calcium in Bulk Drugs and in Pharmaceutical Formulations

Three simple, sensitive and cost effective Spectrophotometric methods are described for the determination of pitavastatin calcium (PST) in bulk drugs and in pharmaceutical formulations. These methods are based on the oxidation of PST by ferric chloride in presence of o-phenanthroline (Method A) or 2, 2’ bipyridyl (Method B) or potassium ferricyanide (Method C). The colored complex formed was measured at 510, 530 and 755 nm for method A, B and C respectively against the reagent blank prepared in the same manner. The optimum experimental parameters for the color production are selected. Beer’s law is valid with in a concentration range of 4-20 μg mL-1 for method A, 7.5-37.5 μg mL-1 for method B and 5 -25 μg mL-1 for method C. For more accurate results, ringbom optimum concentration ranges are 5-18 μg mL-1 for method A , 8.5-35.5 μg mL-1 for method B and 6.0-23.0 μg mL-1 for method C. The molar absorptivities are 3.55x104, 2.10x104 and 3.10x104 L mol-1 cm-1. Where as sandell sensitivities are 0.024, 0.041 and 0.028 μg cm-22 for method A, B and C respectively. The mean percentage recoveries are 99.95 for method A, 101.35 for method B and 100.33 for method C. The developed methods were applied for the determination of PST in bulk powder and in the pharmaceutical formulations without any interference from tablet excipients.

STATISTICAL CORRELATION AND SIMULTANEOUS ESTIMATION OF ATAZANAVIR SULFATE AND RITONAVIR IN FIXED DOSAGE FORM BY HIGH PERFORMANCE LIQUID CHROMATOGRAPHY AND HIGH PERFORMANCE THIN LAYER CHROMATOGRAPHY

Two chromatographic methods are developed and validated to estimate Atazanavir Sulfate and Ritonavir in new fixed dosage form, that is, tablet dosage form named Synthivan. The first method is based on HPLC separation of the two drugs on the reversed phase HiQSil C18 column (5 µm, 250 × 4.6 mm) at ambient temperature using an isocratic solvent system consisting of acetonitrile and water in the ratio 52:48 (v/v). Quantification is achieved with a PDA detector at 254 nm at a flow rate of 1.5 mL/min. Linearity of concentrations is found at 60–600 µg/mL and 20–200 µg/mL for Atazanavir sulfate and ritonavir, respectively. The second method is based on HPTLC separation of the two drugs on pre-coated silica gel 60F254 aluminum plates using toluene:methanol:glacial acetic acid:ethyl acetate (7:0.5:1.5:2, v/v/v/v) as solvent system followed by densitometric measurements of their spots at 254 nm. The linearity of the concentration is found to be 30–300 and 10–100 ng/spot for Atazanavir Sulfate and Ritonavir, respectively. Both methods are validated according to ICH guidelines. The analysis of variance (ANOVA) and Students t-test are applied to correlate the results of Atazanavir Sulfate and Ritonavir determination in dosage form by means of HPLC and HPTLC method.

Development, Validation and Statistical Correlation of RP–LC Methods for Determination of Atazanavir Sulfate in Capsule Dosage Form

To study the effective therapeutic bioavailability of Atazanavir Sulfate (ATV), administered singly or in combination with Ritonavir, a cost effective and rapid method is required. In order to assess an in-depth study, it is primarily thought prudent to develop an effective analytical method for estimation of ATV in marketed dosage forms. The present work is to develop a simple and precise analytical method for in depth evaluation of therapeutic efficacy of ATV. The novelty of the method shows linearity in the concentration range of 10-100 µg/mL at two wavelengths, i.e. 254 nm and 284 nm respectively. The chromatographic system consists of HiQSil C18HS column; an isocratic mobile phase consisted of methanol and tetrahydrofuran (95:5 v/v). The developed method is validated according to ICH guidelines in capsule dosage form. Validation of the developed method shows good result in range, linearity, accuracy and precision. Student’s t–test was used to correlate the two methods and applied to raw materials and capsule dosage form.

Spectrophotometric method for determination of atazanavir sulfate in capsule dosage form

1used in the treatment of human immunodeficiency virus (HIV) Type II infection. ATV is re ported as poorly water soluble and a known substrate for both hepatic metabolizing enzyme Cytochrome 450 (CYP3A) and intestinal drug efflux pump, P-glycoprotein (Pgp) so have low oral bioavailability. 2 So co-administration of small dose of Ritonavir (RTV) is recommended as booster. This new drug is official in IP - 2010, but not included in BP or USP. The reported analytical methods for the determination of ATV are based on high performance liquid chromatography (HPLC) 3-12 in biological samples like blood plasma, biological cells, cerebrospinal fluid (CSF) and blood serum. Stress degradation studies were reported analysed by HPLC and ultraviolet spectrophotometry. 13, 14 The present work was aimed to develop a visible spectrophotometric method, which is simple, sensitive, accurate and cost effective to evaluate the quality of the bulk and pharmaceutical formulations. The novelties of the developed methods are that the reagents used in both the methods are easily available and the mechanisms of reactions of the reagents are already well established. The reactions involved with these reagents are simple, rapid and sensitive. Spectrophotometric methods involve simple instrumentation which is cost effective as compared to other instrumental techniques. The present method involves the determination of ATV, which is a second line drug for treatment of type II HIV infection. Still now, the 2 nd line drugs are available at higher price, than the 1 st line drugs. The high

Comparative study of chromatographic, spectrophotometric and non aqueous titrimetric methods for determination of protease inhibitor in tablets

The paper describes HPLC, UV spectrophotometric and non aqueous titrimetric method for the estimation of poorly water soluble protease inhibitor. Ritonavir in raw material and tablet dosage form. HPLC analysis was carried out in a C18 column using acetonitrile, methanol, and buffer in the ratio 60: 20: 20 (v/v/v) at 240 nm. For the spectrophotometric determination, methanolic solution of Ritonavir was reacted with 3-methyl benzothiazolin-2-one hydrazone (MBTH). The oxidative coupled green coloured chromogen was analysed at 633 nm. Non aqueous titration was carried out using perchloric acid as titrant and the end point was determined using crystal violet as indicator. The three methods were validated and statistically evaluated to correlate the difference between the methods for estimation of Ritonavir in pharmaceutical dosage form.

Densitometric thin-layer chromatography of protease inhibitors in pharmaceutical preparations

Atazanavir sulfate (ATV) (3S,8S,9S,12S)-3,12-bis(1,1dimethylethyl)-8-hydroxy-4,11-dioxo-9-(phenylmethyl)-6-[[4(2-pyridinyl)phenyl]methyl]-2,5,6,10,13-pentaazatetradecanedioic acid dimethyl ester(Figure 1), an azapeptide, is the 7th protease inhibitor used in the treatment of human immunodeficiency virus (HIV) Type II infection [1]. ATV is reported as poorly water soluble and a known substrate for both hepatic metabolizing enzyme Cytochrome 450 (CYP3A) and intestinal drug efflux pump, P-glycoprotein (Pgp), so it has low oral bioavailability [2]. In literature, several methods of analysis are reported for determination of ATV in blood plasma, biological cells, and cerebrospinal fluid by high-performance liquid chromatography (HPLC) [3–12]. Stress degradation studies were reported and analyzed by HPLC and ultraviolet spectrophotometry [13, 14].