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Research Journals >
Indian Journal of Chemical Technology (IJCT) >
IJCT Vol.12 [2005] >
IJCT Vol.12(4) [July 2005] >
| Title: | Sensitive micro analysis of frusemide (furosemide) in bulk drug and formulations by visible spectrophotometry and high performance liquid chromatography (HPLC) |
| Authors: | Basavaiah, K
Chandrashekar, U |
| Keywords: | Frusemide
assay
spectrophotometry
HPLC
prussian blue
formulations |
| Issue Date: | Jul-2005 |
| Publisher: | CSIR |
| IPC Code: | B01D15/00; A61K |
| Abstract: | Two rapid and
sensitive methods using visible spectrophotometry and HPLC are described for
the determination of frusemide (FRU) in bulk drug and formulations.
Spectrophotometry is based on a redox reaction involving FRU followed by
complexation reaction and uses iron(III) and ferricyanide(III) as reagents. The
resulting Prussian blue is measured at
760 nm. The HPLC determination was carried out on a reversed phase Accurasil
ODS C18 column (250  4.6 mm,
5 mm) using a mobile phase consisting of acetonitrile – 0.1%
orthophosphoric acid (pH 3) (60 + 40) at a flow rate of 1.0 mL min-1
with UV detection at 233 nm. Working conditions of both methods have been optimized
and the methods validated as per the ICH guidelines. In spectrophotometry, a
regression analysis of Beer’s law plot showed a good correlation in the
concentration range 0.4 - 4.0  g mL-1
with an apparent molar absorptivity of 4.03 104 L mol-1 cm-1 and a Sandell
sensitivity of 7.85 ng cm-2. The limits of detection and
quantification were calculated to be 0.09 and 0.28 g mL-1 respectively. The linear range of determination by
HPLC was 1.01 - 121.8 g mL-1.
The detection limit (S/N = 3) and quantification limit (S/N = 10) were found to
be 0.3 and 0.6 g mL‑1, respectively.
Within-day accuracies and precisions were £ 3% and between-days precisions were less than 5% for all the
concentrations tested. The methods were applied to the assay of FRU in tablets
and injections. The label claim percentages and relative standard deviations
were in the 98.28- 103.24 and 0.36 - 2.04% range, respectively. The validity of
the methods was further ascertained by parallel determination by a reference
method and by recovery studies via standard addition technique. The results
showed that the procedures are suitable for routine analysis of the diuretic. |
| Page(s): | 401-406 |
| ISSN: | 0975-0991 (Online); 0971-457X (Print) |
| Source: | IJCT Vol.12(4) [July 2005]
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