Фармацевтика Аналитика Акта

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A Validated HPLC Method for the Determination of Tiludronate Disodium on a Novel Brominated Stationary Phase

Wagdy HA, Bowser JE, Tarek M and Aboul-Enein HY

An analytical method for analysis of Tiludronate; [4-chlorothiophenyl) methylene] bisphosphonate known as Tildren® is developed without pre or post derivatization on a newly introduced halogenated stationary phase namely pentabromobenzyl column (PBr column) for the first time.

The optimum HPLC conditions used are: A mobile phase composed of acetonitrile: Water: triethylamine: Acetic acid (50: 50: 0.05: 0.05; v: v: v: v), at a flow rate 0.5 mL/min, at temperature 35°C. Two wavelengths were selected from the UV-spectrum namely 197 and 267 nm.

The method is linear in the range of 0.06-0.6 mg/mL with square of the regression coefficient (r2) 0.9998 at 197 nm. The limit of quantification (LOQ) is 0.040 mg/mL and the limit of detection (LOD) is 0.013 mg/mL. The method is precise with %RSD 0.41-1.36 (intra-day) and %RSD 0.38-1.91 (inter-day). The method is found to be robust at temperature 35°C ± 3°C, wavelength 197 nm ± 1 nm, pH of the aqueous phase ± 0.03 and %ACN 50% ± 1%.

At 267 nm, the method is linear in the range of 0.08-0.8 mg/mL with r2 0.9997, LOQ is 0.050 mg/mL and LOD is 0.016 mg/mL. The %RSD for intra-day precision ranges from 0.96-1.74, while for inter-day precision ranges from 1.09-2.32. The method is proved robust in temperature 35°C ± 3°C, wavelength 297 nm ± 3 nm, pH of the aqueous phase ± 0.03 and %ACN 50% ± 1%.

The method is accurate with % recovery ranged from 98.82-99.42% with %RSD ranging from 0.210-1.023.

This method is suitable for the assay of tiludronate in both bulk and in its veterinary pharmaceutical formulations.