Spectrophotometric determination of sparfloxacin in tablets

J. Antimicrob Chemother 1999; 43: 136–137

Hérida R. N. Maronaa,* and Elfrides E. S. Schapovalb

a Faculdade de Ciências Farmacêuticas, UNESP, Rod. Araraquara-Jaú, km 1, CEP. 14801-902, Araraquara, SP b Curso de Pós-graduação em Ciências Farmacêuticas, UFRGS, Av. Ipiranga, 2752, Porto Alegre, CEP. 90610-000, RS, Brazil

Sir,

Sparfloxacin is a fluoroquinolone antibacterial agent active against Gram-positive and Gram-negative bacteria. 1,2 It has been reported to be more active in vitro than other quinolones against some microorganisms including staphylococci and mycobacteria, 3,4 and has a 16 h plasma half-life. 5 High-performance liquid chromatography methods for the analysis of sparfloxacin in body fluids have been reported, 6,7 but there is no information on the quantification of sparfloxacin in tablets. This report describes a sensitive and accurate spectrophotometric method for determination of sparfloxacin in raw material and tablets.

Sparfloxacin powder (99.5% potency) was supplied by Dainippon Pharmaceutical Co. (Osaka, Japan). Each sparfloxacin tablet contained 200 mg of the active drug. The sparfloxacin powder and tablets were stored protected from light. Solutions of sparfloxacin powder in methanol (1 mg/mL) were prepared by accurately weighing 10 mg of sparfloxacin into a 50 mL volumetric flask, adding 10 mL methanol and shaking for 30 min by mechanical shaker, followed by sterile distilled water up to volume. The sparfloxacin standard solution was diluted in 50 mL volumetric flasks with sterile distilled water to give a range of solutions with final concentrations of 2–12 mg/L. The absorbance value of each solution at 292 nm was determined in a 10 mm quartz cell using a UV–VIS spectrophotometer (Shimadzu, Kyoto, Japan). To analyse the concentratrion of sparfloxacin in tablets, each tablet was weighed to obtain the average tablet weight. The tablets were ground up and 960 mg (representing three times the average weight of each tablet) was transferred to a 1000 mL volumetric flask; 200 mL methanol was added and the flask was shaken for 30 min by mechanical shaker followed by addition of sterile distilled water to volume. Aliquots of 10 mL of this solution were transferred to a 100 mL volumetric flask and sterile distilled water was added to volume to give an estimated concentration of 60 mg/L. After rotation in a centrifuge flask, the solution was diluted 1:10 to give a final estimated concentration of 6.0 mg/L. This solution was prepared six times and the absorbance of each solution was determined at 292 nm. In addition, to verify the accuracy of the tablet solutions, a standard solution of 200 mg/L made from sparfloxacin powder was added in 1, 2 and 3 mL aliquots to sample solutions with 600 mg/L to give a final estimated concentration of 8, 10 and 12 mg/L, respectively. The most powerful statistical tool to verify the internal validity of an analytical procedure, a criterion of accuracy, is the analysis of variance (ANOVA). Therefore, the data were analysed by linear simple regression by the least-squares method using Excel 5.0.

The aim of this study was to develop a spectrophotometric procedure for the analysis of sparfloxacin in raw material and tablets. The linear regression equation for sparfloxacin was calculated to be y = 0.0725x + 0.0008, where x and y are concentration and absorbance, respectively. The method had excellent reproducibility for the standard solution of 100 mg/L, 97.08 ± 1.07% (n = 6). The recovery test is an experimental design to verify the relationship between the amount of substance added and the amount quantified by this assay. In this test the observed concentrations of pure sparfloxacin in the powdered tablets were not significantly different from the stated concentrations by Student's t test, P = 0.05% (100.04 ± 1.39%, n = 3). The detailed accuracy and precision data are shown in the Table. The method gave rise to linear data in the range 2–12 mg/L with accuracy and precision in the range 0.56–3.01%. Therefore, this UV-spectrophotometric assay was accurate, and may be recommended for the simple quantification of sparfloxacin.


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Table. Experimental values obtained in the recovery test for sparfloxacin in tablets
 

Acknowledgments

The authors are grateful to Dr Sayuri Kitada (Dainippon Co., Japan) and Dr Michael Pease (Rhône-Poulenc Rorer, Collegeville, PA, USA) for providing the sparfloxacin reference substance, and to Helder Teixeira for providing the tablets. This work was financed by a CAPES/PICDT programme.

Notes

* Corresponding author. Fax: +55-51-316-5437; E-mail: hmarona{at}hotmail.com Back

References

1 . Chin, N. X., Gu, J. W., Yu, K. W., Zhang, Y. X. & Neu, H. C. (1991). In vitro activity of sparfloxacin. Antimicrobial Agents and Chemotherapy< 35, 567–71.[ISI][Medline]

2 . Miyamoto, T., Matsumoto, J. I., Chiba, K., Egawa, H., Shibamori, K., Minamida, A. et al. (1990). Synthesis and structure activity relationships of 5-substituted 6,8 fluoroquinolones, including sparfloxacin, a new quinolone antibacterial agent with improved potency. Journal of Medicinal Chemistry 33, 1645–56.[ISI][Medline]

3 . Perrone, C., Gikas, A., Truffot-Pernot, C., Grosset, J., Vilde, J. L. & Pocidalo, J. J. (1991). Activities of sparfloxacin, azithromycin, temafloxacin, and rifapentine compared with that of clarithromycin against multiplication of Mycobacterium avium complex within human macrophages. Antimicrobial Agents and Chemotherapy 35, 1356–9.[ISI][Medline]

4 . Rastogi, N. & Goh, K. S. (1989). In vitro activity of the new difluorinated sparfloxacin against Mycobacterium tuberculosis compared with activities of ofloxacin and ciprofloxacin. Antimicrobial Agents and Chemotherapy5, 33–6.

5 . Shimada, J., Nogita, T. & Ishibashi, Y. (1993). Clinical pharmacokinetics of sparfloxacin. Clinical Pharmacokinetics 25, 358–69.[ISI][Medline]

6 . Borner, K., Borner, E. & Lode, H. (1992). Determination of sparfloxacin in serum and urine by high-performance liquid chromatography. Journal of Chromatography and Biomedical Applications 579, 285–9.

7 . El-Sayed, Y. M. (1995). A simple high-performance liquid chromatographic assay for sparfloxacin in human plasma. Analytical Letters 28, 279–93.[ISI]





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