Fourth‐derivative synchronous spectrofluorimetry and HPLC with fluorescence detection as two analytical techniques for the simultaneous determination of itopride and domperidone

Abstract

Two simple, rapid and sensitive methods, namely, fourth-derivative synchronous spectrofluorimetry (method I) and HPLC with fluorescence detection (method II) were developed for the simultaneous analysis of a binary mixture of itopride HCl (ITP) and domperidone (DOM) without prior separation. The first method was based on measuring the fourth derivative of the synchronous fluorescence spectra of the two drugs at Δλ = 40 nm in methanol. The different experimental parameters affecting the synchronous fluorescence of the studied drugs were carefully optimized. Chromatographic separation was performed in < 6.0 min using a RP C18 column (250 mm × 4.6 mm i.d., 5 µm particle size) with fluorescence detection at 344 nm after excitation at 285 nm. A mobile phase composed of a mixture of 0.02 M phosphate buffer with acetonitrile in a ratio of 55 : 45, pH 4.5, was used at a flow rate of 1 mL/min. Linearity ranges were found to be 0.1-2 µg/mL for ITP in both methods, whereas those for DOM were found to be 0.08-2 and 0.05-1.5 µg/mL in methods I and II, respectively. The proposed methods were successfully applied for the determination of the studied drugs in synthetic mixtures and laboratory-prepared tablets.

Liquid chromatographic and spectrofluorimetric assays of empagliflozin: Applied to degradation kinetic study and content uniformity testing

“…The spectrofluorimetric scan for EGF showed excitation and emission spectra at 226.5 and 299.4 nm, respectively (Figures and a) because of the conjugated system that appears in its structure (Figure ). In the underlying investigation, synchronous technique was used applying ∆ λ = 70 nm with enhanced sensitivity and features bands at 297.6 nm as shown in Figure (b). A marked decrease in spectra overlapping and marked increase in linearity parameters confirmed the advantages of using synchronous technique over the conventional spectrofluorimetric analysis.…”

“…The spectrofluorimetric scan for EGF showed excitation and emission spectra at 226.5 and 299.4 nm, respectively (Figures 3 and 4a) because of the conjugated system that appears in its structure ( Figure 1). In the underlying investigation, synchronous technique was used applying Δλ = 70 nm with enhanced sensitivity and features bands [27][28][29][30][31] at 297.6 nm as shown in Figure 4…”

“…Furthermore, to save the time consuming method development that is usually used to adjust the excitation and emission wavelengths and to face the problem of broad spectra, synchronous technique was conducted with simple runs, enhanced resolution and better regression parameters. Synchronous technique had been used for analysis of many pharmaceutical products because of its advantages over the conventional mode …”

“…Synchronous technique had been used for analysis of many pharmaceutical products because of its advantages over the conventional mode. [27][28][29][30][31] [4] Direct UV Methanol and water 2-6 277 nm Determination of EGF and LIG in tablets [5] Simultaneous equation Methanol and water 6-12 277 nm Determination of EGF and LIG in tablets [5] First derivative Methanol 2.5-30 221 and 238 nm Determination of EGF and LIG in tablets [6] Simultaneous equation Methanol 2-12 225 and 237 nm Determination of EGF and MRN in tablets [7] PLS-2 Methanol 2-10 200-300 nm Determination of EGF and MRN in tablets [7] Simultaneous equation Methanol 2-25 272 and 234 nm Determination of EGF and MRN in tablets [8] Absorption ratio Methanol 2-25 254 and 226 nm Determination of EGF and MRN in tablets [8] First derivative Methanol 2-12 223.5 and 233.5 nm Determination of EGF and MRN in tablets [9] Direct UV Water 2-12 247 nm Determination of EGF in tablets [10] Phenanthroline reaction Water 5-30 438 nm Determination of EGF in tablets [10] K Ferricyanide reaction Water 10-60 782 nm Determination of EGF in tablets [10] Derivative ratio Methanol 2-12 230 and 242 nm Determination of EGF and MRN in tablets [11] Ratio subtraction Methanol 2-12 237 nm Determination of EGF and MRN in tablets [11] Ext. ratio subtraction Methanol 2-12 225 nm Determination of EGF and MRN in tablets [11] Direct UV Methanol 5-25 296 nm Determination of LIG with EGF and MRN [12] Mean centering Methanol 2-12 222 and 249 nm Determination of EGF and MRN in tablets [13] First derivative Methanol 5-25 310 nm Determination of LIG with EGF and MET [14] Spectrum subtraction Methanol 2-12 225 nm Determination of EGF and MRN in tablets [15] Constant multiplication Methanol 2-12 237 nm Determination of EGF and MRN in tablets [15]…”

Second‐derivative synchronous spectrofluorimetric assay of dapagliflozin: Application to stability study and pharmaceutical preparation

“…SFS can also provide a more selective method for drug analysis, without the need to use a separation technique such as high performance liquid chromatography . The use of a derivative technique, along with SFS, would provide a sensitive analytical method compared with conventional native fluorescence techniques . The proposed analytical method was suitable for DGF assay under stress conditions.…”