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  • Author: Kanakapura Basavaiah x
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Pavagada Ramesh, Kanakapura Basavaiah and Nagaraju Rajendraprasad

Sensitive and selective spectrophotometric assay of doxycycline hyclate in pharmaceuticals using Folin-Ciocalteu reagent

A spectrophotometric method for the determination of doxycycline (DOX) is described. The method is based on the formation of blue colored chromogen due to reduction of tungstate and/or molybdate in Folin-Ciocalteu (F-C) reagent by DOX in alkaline medium. The colored species has an absorption maximum at 770 nm and the system obeys Beer's law over the concentration range 0.75-12.0 μg mL-1 DOX. The apparent molar absorptivity is 2.78 × 104 L mol-1 cm-1. The limit of quantification and detection values are reported to be 0.20 and 0.08 μg mL-1, respectively. Over the linear range applicable, the accuracy and precision of the method were evaluated on intra-day and inter-day basis. The reported mean accuracy value was 101.0 ± 1.7 %, the relative error was ≤ 2.7 % and the relative standard deviation was ≤ 2.5 %. Application of the proposed method to bulk powder and commercial pharmaceutical tablets is also presented. No significant difference was obtained between the results of the proposed method and the official BP method. The procedure described in this paper is simple, rapid, accurate and precise.

Open access

Kanakapura Basavaiah, Hullikal Prameela and Bankavadi Somashekar

Spectrophotometric determination of pefloxacin mesylate in pharmaceuticals

A spectrophotometric method is described for assay of pefloxacin mesylate (PFM) in bulk drug and in tablets. The method is based on back extraction of the bromophenol blue dye at pH 5.2 from the dye-drug ion pair followed by measurement of the dye absorbance at 590 nm. The working conditions of the method were investigated and optimized. Beer's law plot showed a good correlation in the concentration range of 0.15-1.25 μg mL-1. Sensitivity indices such as molar absorptivity, limits of detection and quantification are reported. Intra-day and inter-day precision, and accuracy of the methods were established according to the ICH guidelines, and the e r values were in the range of -1.7 to 1.8% with RSD values ranging from 1.0 to 1.1%. The method was successfully applied to the assay of PFM in tablet preparations with recoveries varying from 97.5 to 101.9%, with standard deviation in the range of 0.6 to 1.9. The results were statistically compared with those of the reference method by applying Student's t-test and F-test. Accuracy evaluated by means of the spike recovery method, range from 97.0 to 106.0%, with precision better than 3%.

Open access

Kanakapura Basavaiah, Urdigere Anil Kumar and Kalsang Tharpa

Gradient HPLC analysis of raloxifene hydrochloride and its application to drug quality control

A rapid, sensitive and selective method for the determination of raloxifene hydrochloride (RLX) in pure drug and in tablets was developed using gradient high performance liquid chromatography (HPLC). The devised method involved separation of RLX on a reversed phase Hypersil ODS column and determination with UV detection at 284 nm. The standard curve was linear (R = 0.999) over the concentration range of 50--600 μg mL-1 with a detection limit of 0.04 μg mL-1 and a quantification limit of 0.16 μg mL-1. Intra-day and inter-day precision and accuracy of the method were established according to the current ICH guidelines. Intra-day RSD values at three QC levels (250, 450 and 550 μg mL-1) were 0.2--0.5%, based on the peak area. The intra-day relative error (e r) was between 0.2 and 0.5%. The developed method was successfully applied to the determination of RLX in tablets and the results were statistically compared with those obtained by a literature method. Accuracy, evaluated by means of the spike recovery method, was the excellent with percent recovery in the range 97.7--103.2 with precision in the range 1.6--2.2%. No interference was observed from the co-formulated substances. The method was economical in terms of the time taken and the amount of solvent used.

Open access

Kanakapura Basavaiah, Veeraiah Ramakrishna and Urdigere Kumar

Use of ceric ammonium sulphate and two dyes, methyl orange and indigo carmine, in the determination of lansoprazole in pharmaceuticals

Two spectrophotometric methods are proposed for the assay of lansoprazole (LPZ) in bulk drug and in dosage forms using ceric ammonium sulphate (CAS) and two dyes, methyl orange and indigo carmine, as reagents. The methods involve addition of a known excess of CAS to LPZ in acid medium, followed by determination of residual CAS by reacting with a fixed amount of either methyl orange, measuring the absorbance at 520 nm (method A), or indigo carmine, measuring the absorbance at 610 nm (method B). In both methods, the amount of CAS reacted corresponds to the amount of LPZ and the measured absorbance was found to increase linearly with the concentration of LPZ, which is corroborated by the correlation coefficients of 0.9979 and 0.9954 for methods A and B, respectively. The systems obey Beer's law for 0.5-7.0 μg mL-1 and 0.25-3.0 μg mL-1 for methods A and B, respectively. The apparent molar absorptivities were calculated to be 3.0 x 104 and 4.4 x 104 L mol-1 cm-1 for methods A and B, respectively. The limits of detection (LOD) and quantification (LOQ) were calculated to be 0.08 and 0.25 μg mL-1 for method A, and 0.09 and 0.27 μg mLs-1 for method B, respectively. The intra-day and inter-day precision and accuracy of the methods were evaluated according to the current ICH guidelines. Both methods were of comparable accuracy (e r ≤ 2 %). Also, both methods are equally precise as shown by the relative standard deviation values < 1.5%. No interference was observed from common pharmaceutical adjuvants. The accuracy of the methods was further ascertained by performing recovery studies using the standard addition method. The methods were successfully applied to the assay of LPZ in capsule preparations and the results were statistically compared with those of the literature UV-spectrophotometric method by applying Student's t-test and F-test.

Open access

Kanakapura Basavaiah, Bankavadi Somashekar and Veeraiah Ramakrishna

Rapid titrimetric and spectrophotometric methods for salbutamol sulphate in pharmaceuticals using N-bromosuccinimide

One titrimetric and two spectrophotometric methods which are simple, sensitive and rapid are described for the assay of salbutamol sulphate (SBS) in bulk drug and in tablet dosage forms using N-bromosuccinimide (NBS) and two dyes, rhodamine-B and methylene blue, as reagents. In titrimetry, aqueous solution of salbutamol sulphate is treated with a measured excess of NBS in acetic acid medium and after the oxidation of SBS is complete, the unreacted oxidant is determined iodometrically. Spectrophotometric methods entail addition of a known excess of NBS in acid medium followed by the determination of residual oxidant by reacting with a fixed amount of either rhodamine B and measuring the absorbance at 555 nm (method A) or methylene blue and measuring the absorbance at 665 nm (method B). In all methods, the amount of NBS reacting corresponds to the amount of SBS content. Titrimetric method is applicable over 1.74 x 10-4 - 8.68 x 10-4 mol L-1 range and the reaction stoichiometry is found to be 1:6 (SBS:NBS). In spectrophotometric methods, the absorbance is found to increase linearly with the concentration of SBS, which is corroborated by the correlation of coefficients of 0.9993 and 0.9988 for method A and method B, respectively. The systems obey Beer's law for 0.25-1.75 μg mL-1 (method A) and 0.5-5.0 μg mL-1 (method B). The calculated apparent molar absorptivity values were found to be 2.10 x 105 and 6.16 x 104 L mol-1 cm-1, for method A and method B, respectively. The limits of detection and quantification are also reported for both spectrophotometric methods. Intraday and inter-day precision and accuracy for the developed methods were evaluated. The methods were successfully applied to the assay of SBS in tablet and capsule formulations and the results were statistically compared with those of a reference method. No interference was observed from common tablet adjuvants. The accuracy and reliability of the methods were further ascertained by recovery experiments via the standard-addition technique.