Abstract
Five simple, sensitive, accurate and precise methods were developed for determination of raloxifene (RLX) in pure form as well as in its pharmaceutical preparation. Method [A] is HPLC stability–indicatingmethod, where the intact drug (RLX), the internal standard (methocarbamol) and RLX degradation products were separated using a YMC-pack ODS-AQ C18 column (150 mm X 4.6 mm ID, 3µm particle size ) using acetonitrile–0.05 M KH2PO4 adjusted to pH 2.5 using H3PO4 (50 : 50 v/v ) as a mobile phase at a flow rate 1 ml/min. and UV detection at 280 nm, where a good linearity was obtained in the range of 0.5 – 8 µgml-1.The LOD was 0.077 µg ml-1 and the LOQ was 0.258 µgml-1. Method [B] depended on measurement of the difference absorbance (ΔA) of the drug in the presence of its degradate between solutions in methanolic 0.1 M HCl and 0.1 M NaOH at 285 nm. Beer’s low was obeyed in the range of 3 – 27 µgml-1. LOD and LOQ were found to be 0.233 and 0.778 µg ml-1,respectively. Method [C] is stability – indicating First-Derivative (1D) for the determination of intact RLX in presence of its degradation product at 268 nm in the range of 3 – 18 µg ml-1 with LOD of 0.254 µg ml- and LOQ of 0.849 µg ml-1. Method [D] depended on ion pairing of RLX with eosin-Y dye at pH 3.5 to produce red coloured complex measured at 545 nm. Beer’s low was obeyed in the range of 2 – 20 µgml-1. LOD and LOQ were found to be 0.276 and 0.920 µg ml-1,respectively. Method [E] depended on ion pairing of RLX with bromothymol blue (BTB) dye at pH 2.6 to form a chloroform-soluble coloured ion association complex. The formed complex could be extracted and measured at 420 nm. Good agreement with Beer’s low was found in the range of 4 – 28 µgml-1. LOD and LOQ were found to be 0.633 and 2.110 µg ml-1,respectively. The percent recoveries ± RSD% of these methods were 100.83±0.920, 100.24±0.724, 100.15±0.586, 100.26±0.383 and 99.98±0.261, respectively. The obtained results were compared with those of the reported method and no significant difference was observed regarding accuracy and precision.
Highlights
Raloxifene hydrochloride (RLX), 6-Hydroxy-2-(p-hydroxyphenyl) benzo[b]thien-3-ylp-(2-piperidinoethoxy) phenyl ketone hydrochloride, is a second generation selective estrogen receptor modulator
For method E (Ion-Pair Technique with bromothymol blue (BTB)): Into a series of 125 ml separating funnels, transfer aliquot portions of the standard drug solution (0.1 mg ml-1) containing (0.1 – 0.7 mg), add 4 ml of phthalate buffer pH 2.6 followed by 3 ml of BTB (0.1%).Adjust the total volume of the aqueous phase to 15 ml by the addition of water, shake the contents for about one minute
Analysis of pharmaceutical preparation: For method A, five tablets of Evista® 60 mg were weighed and finely powdered, an accurately weighed amount of powder equivalents to 10 mg, dissolved in the least amount of methanol, completing the volume to 50 ml with mobile phase, filtered into 100 ml volumetric flask and the volume was completed with the mobile phase
Summary
Raloxifene hydrochloride (RLX), 6-Hydroxy-2-(p-hydroxyphenyl) benzo[b]thien-3-ylp-(2-piperidinoethoxy) phenyl ketone hydrochloride, is a second generation selective estrogen receptor modulator. For method A (HPLC Technique): Stock solution of the drug (0.1 mg ml-1) was prepared by dissolving 10 mg powder in the least amount of methanol completing the volume to 100 ml with mobile phase. For method B (ΔA Technique): Two stock solutions of RLX (0.1 mg ml-1) were prepared by dissolving 10 mg powder in 100 ml of 0.1 M methanolic HCl and 100 ml of 0.1 M methanolic NaOH. For method C (First-Drivative Technique): Standard solution of RLX (0.05 mg ml-1) was prepared by dissolving 5 mg of the drug in methanol and completing the volume to 100 ml with the same solvent. For methods D and E (Ion-Pair Technique): 10 mg of RLX powder was accurately weighed and transferred into 100 ml volumetric flask, dissolved in the least amount of ethanol, the volume was completed to the mark with water to obtain ( 0.1 mg ml-1 ).
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