Simultaneous Determination of Salmeterol Xinafoate and Fluticasone Propionate in Bulk Powder and SeritideDiskus using High Performance Liquid Chromatographic and Spectrophotometric Method

Abstract

Five methods were developed for simultaneous determination of Salmeterol xinafoate (SAM) and Fluticasone propionate (FLU) without previous separation. In the first method (HPLC), a reversed-phase column and a mobile phase of acetonitrile: methanol (80:20 v/v) at 0.5 mLmin-1 flow rate was used to separate both drugs and UV detection at 220 nm. Linearity was obtained in concentration ranges of 50-500 µgmL-1 for Salmeterol xinafoate Fluticasone propionate. In the second method both drugs were determined using first derivative UV spectrophotometry, with zero crossing measurement at 352 and 269.5 nm for Salmeterol xinafoate and Fluticasone propionate, respectively. The third method depends on first derivative of the ratios spectra by measurements of the amplitudes at 334 and 337.5 nm for Salmeterol xinafoate and at 225 and 231.5 nm for Fluticasone propionate. Calibration graphs were established in the range of 4-28 µgmL-1 for both Salmeterol xinafoate and Fluticasone propionate. The fourth one depend on isosbestic point at 237.5 nm, while the content of Salmeterol xinafoate was determined by measuring the absolute value of the ultraviolet curves at 343 nm, without interference from Fluticasone propionate. All the proposed methods were extensively validated. They have the advantage of being economic and time saving. All the described methods can be readily utilized for the analysis of pharmaceutical formulations. The results obtained by adopting the proposed methods were statistically analyzed and compared with those obtained by official methods.

Method Development and Validation of the Chromatographic Analysis of Fluticasone Propionate and Salmeterol Xinafoate Combination in Solutions and Human Plasma Using HPLC With Uv Detection

“…For example, in a previous study, an X-terra column (250 mm x 4.6 mm, 5 µm) was used to elute FP and SX with mobile phase consisted of Methanol: Acetonitrile: Water (50:35:15 % v/v) at 1 ml/min flow rate [12]. In other reported methods Acetonitrile: Methanol, Methanol: Water, buffered or modified mobile phases with different types of columns were used [9,11,26,[28][29][30][31][32].…”

“…Several chromatographic techniques have been published in the literature for analysis purposes of fluticasone propionate (FP) and/or, salmeterol xinafoate (SX) in their pharmaceutical preparations and different matrices. For example these methods include UVspectrometric methods [6,7], HPLC with UV detection methods [8][9][10][11][12][13], HPLC-MS/MS methods [14,15], UPLC-MS/MS methods [16,17], UPLC-PDA method [18], and HPTLC method [19,20].…”

Quantitative proton nuclear magnetic resonance method for simultaneous analysis of fluticasone propionate and azelastine hydrochloride in nasal spray formulation

“…Reviewing the literature revealed that different analytical methods were established for determination of FLP and AZH either alone or in combination. These methods include: spectrophotometry [5][6][7][8][9][10][11][12], spectrofluorometry [13,14], electrochemical methods [15][16][17], TLC [18,19], HPLC [5,11,[20][21][22][23][24][25][26][27][28][29]] HPTLC [30][31][32], LC/MS/MS [33][34][35][36][37][38][39] and capillary electrophoresis [40,41]. It was found that only two spectrophotometric methods [42,43] and two HPLC methods [44,45] were reported for quantification of the binary mixture of FLP and AZH.…”

HPLC method for simultaneous determination of salmeterol xinafoate and fluticasone propionate for the quality control of dry powder inhalation products

“…Thus, the methods with LLOQ above 0.1 μg mL −1 are not suitable for monitoring the invitro deposition pattern. Moreover, in some methods, the quantitation limit had not been provided [6] or only theoretical values of detection limits calculation, based on the standard, were assessed [7]. The methods involving spectrophotometry are widely used in pharmaceutical control laboratories due to their simplicity, low-cost instrumentation, and adaptability.…”

“…Few high-performance liquid chromatography (HPLC) analytical methods have been published so far for SX and FP simultaneous determination in pharmaceutical formulation [3][4][5][6][7]. According to the International Conference on Harmonization guidelines, if a value for the detection limit is obtained by calculation or extrapolation, this estimate should be subsequently validated by an independent analysis of a suitable number of samples known to be near or at the detection limit which has not been the case so far [8].…”