A NOVEL APPLICATION OF IMMOBILIZATION ON MEMBRANES FOR THE SEPARATION AND SPECTROFLUORIMETRIC QUANTIFICATION OF AMILORIDE AND FUROSEMIDE IN PHARMACEUTICAL SAMPLES.

PERALTA, CECILIA; FERNANDEZ, LILIANA; MASI, ADRIANA

ANALYTICA CHIMICA ACTA

Elsevier

Año: 2010 vol. 661 p. 85 - 90

0003-2670

A new, simple and highly sensitive method for spectrofluorimetric determination of amiloride (AMI) and furosemide (FUR) in pharmaceuticals is presented. The proposed method is based on the separation of AMI from FUR by solid-phase extraction using a nylon membrane, followed by spectrofluorimetric determination of both drugs, on the solid surface and the filtered aqueous solution, respectively. AMI shows low native fluorescence, but its separation-preconcentration by immobilization (solid phase extraction) on nylon membrane surface provides a considerable enhancement in fluorescence intensity. The fluorescence determination is carried out at ëex = 237, ëem = 415 nm for FUR; and ëex = 365, ëem = 406 nm for AMI. The calibration graphs are linear in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 415 nm for FUR; and ëex = 365, ëem = 406 nm for AMI. The calibration graphs are linear in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 415 nm for FUR; and ëex = 365, ëem = 406 nm for AMI. The calibration graphs are linear in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 415 nm for FUR; and ëex = 365, ëem = 406 nm for AMI. The calibration graphs are linear in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 carried out at ëex = 237, ëem = 415 nm for FUR; and ëex = 365, ëem = 406 nm for AMI. The calibration graphs are linear in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 and ëex = 365, ëem = 406 nm for AMI. The calibration graphs are linear in the range 3.20 x 10-4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10 -4- 0.8 ìg mL-1and 1.33 x 10-3 - 4.0 ìg mL-1, for AMI and FUR, respectively, with a detection limit of 9.62 x 10-5 and 4.01 x 10-5 and 4.01 x 10 -4 ìg mL-1 (S/N=3). The commonly found excipients in commercial pharmaceutical formulations do not interfere. The developed method is successfully applied to the determination of both drugs in pharmaceutical formulations. interfere. The developed method is successfully applied to the determination of both drugs in pharmaceutical formulations. interfere. The developed method is successfully applied to the determination of both drugs in pharmaceutical formulations. interfere. The developed method is successfully applied to the determination of both drugs in pharmaceutical formulations. ìg mL-1 (S/N=3). The commonly found excipients in commercial pharmaceutical formulations do not interfere. The developed method is successfully applied to the determination of both drugs in pharmaceutical formulations.