Validated Chromatographic and Spectrofluorimetric Methods for Analysis of Silodosin: A Comparative Study with Application of RP-HPLC in the Kinetic Investigation of Silodosin Degradation

Abstract

Background Stability indicating determination of pharmaceuticals is crucial, especially for drugs which have few published official analytical methods. Silodosin (SLD) is an FDA approved α1A-adrenoceptor blocker. Objective Efficient analytical methods were suggested, based on different instrumental techniques for quantification of SLD, besides conducting kinetic investigation of its degradation. Methods The first method is based on Reversed Phase High Performance Liquid Chromatography with Photodiode Array Detector (RP-HPLC-PDAD). Detection is done at wavelength 225 nm. The second method is focused on using High Performance Thin Layer Chromatography (HPTLC) and eluting the drug by solvent mixture followed by scanning at wavelength 270 nm. The third method depends on the First Derivative Synchronous Fluorescence Spectroscopy (1DSFS) for analysis of solutions of SLD and its acid and oxidative induced degradation products at Δλ = 90 nm, then determining the first derivative of the spectra and measuring peak amplitudes at 360 nm. Results Acceptable linearities were found in the concentration range of 0.50–90 μg/mL, 0.10–3.0 μg/band, and 0.05–0.50 µg/mL, for RP-HPLC-PDAD, HPTLC, and spectrofluorimetric methods, respectively. Conclusion Statistical analysis showed no significant difference between the suggested and the reported method. In monitoring the kinetics of SLD degradation, the order of reactions was determined and effects of degrading agent concentration and temperature on reaction rate were studied. Highlights Three analytical methods were developed for the determination of SLD based on RP-HPLC-PDAD, HPTLC, and 1DSFS in bulk and capsule dosage form. In addition, kinetic investigation of SLD degradation was performed using the developed RP-HPLC-PDAD method.

Computational Design and Application of Molecularly Imprinted/MWCNT Based Electrochemical Sensor for the Determination of Silodosin

“…The limit of detection (LOD), calculated based on a signal‐to‐noise ratio (S/N=3) and limit of quantification (LOQ) were found to be 10 −13 and 3.3×10 −13 M equivalent to (4.95×10 −8 and 1.63×10 −7 μg/mL), respectively, which are much lower than those of the previously reported methods in literature for the determination of SLD including: electrochemical, spectrophotometric, spectrofluorimetric, and chromatographic methods [7, 8, 10, 11, 20, 21] as shown in Table 4. Statistical analysis of data was performed using student's t and F‐tests to estimate the variance in the mean of the analysis results in comparison with a standard reference method for the data obtained for the detection on pure SLD and Flopadex® dosage form, as given in Table 5.…”

“…Several methods have been reported for the determination of SDL such as, liquid chromatography with mass spectrometric detection (LC-MS/MS) [2][3][4], liquid chromatography/ Fourier transform mass spectrometry [5], LC-ESI-MS/MS [6], (UPLC/MS/MS) [7,8], UHPLC-QTOF-MS/MS for in silico toxicological screening of its metabolites [9], (RP HPLC) [10][11][12][13][14], micellar electro kinetic chromatography [15], UV-VIS [16,17], charge transfer complex and validated stability-indicating spectrophotometric method [18,19] and spectrofluorimetry [20]. An electrochemical sensor based on Graphene Nanosheets/Gold nanoparticles/Nafion nanocomposite modified glassy carbon electrode was also reported [21].…”

Development and Validation of Novel FTIR Method for Quantitative Estimation of Silodosin in Bulk and Pharmaceutical Dosage Forms

“…According to a literature review [3][4][5][6][7][8][9][10] , methods for estimating Silodosin include HPLC, UV spectrophotometric, and UPLC. Due to the lack of an FTIR method for silodosin estimation, As a result, the current research is an attempt to use FTIR to develop a novel, sensitive method for quantifying silodosin.…”

Analytical reversed‐phase high‐performance liquid chromatography method development for silodosin and solifenacin in bulk and marketed formulation using analytical quality by design approach

“…Chemically SLD is 1-(3-Hydroxypropyl)-5-[(2R)-2-({2-[2-(2, 2, 2-trifluoro Ethoxy) phenoxy l] ethyl} amino) propyl]-2, 3-dihydro-1H-indole-7-carboxamide having molecular formula C 25 H 32 F 3 N 3 O 4 as shown in Figure S1A. SLD is a potent antagonist of post-synaptic alpha adrenoreceptors which are found mainly in the human prostate, the base of the bladder, the neck of the bladder, the urethral capsule, and the prostatic urethra [6,7]. Due to the inhibition of alpha-1 adrenoreceptor, the smooth muscles in these tissues may relax which enhances urine flow and lower the BPH symptoms [8,9].…”