Journal of Analysis and Testing

, Volume 3, Issue 4, pp 322–330 | Cite as

Online Postcolumn Indirect Detection for Determination of Ibandronate in Pharmaceutical Tablets by HPLC/DAD

  • Mokhtar Mabrouk
  • Sherin F. Hammad
  • Mohamed A. Abdelaziz
  • Fotouh R. MansourEmail author
Original Paper


Ibandronate sodium monohydrate is a highly polar aliphatic compound that belongs to the bisphosphonate class, a widely used bone resorption inhibitor. The aliphatic nature of ibandronate precludes direct photometric detection and its high polarity urged analysts to use ion-pairing agents in the mobile phase to promote retention in reversed-phase columns. In this work, a reversed-phase method for determination of ibandronate sodium monohydrate in pharmaceutical tablets is introduced by employing an online postcolumn ligand exchange reaction to enable photometric detection. The method offers for the first time the ability to separate the drug from its well-known impurities on conventional reversed-phase columns. The detection reaction depends on the ability of ibandronate and its degradation products to displace salicylate in the iron(III) salicylate complex, forming various colorless iron (III) complexes and showing a negative chromatographic signal for ibandronate and its degradants at λmax = 525 nm. The chromatographic separation was achieved using a Hypersil BDS C8 column (5 µm particle size, 150 mm × 4.6 mm i.d.) and a mobile phase consisting of a mixture of aqueous formate buffer pH 3 (pH 3, 5 mM) and methanol in a ratio of 80:20% (v/v), delivered at a flow rate of 0.8 mL/min. The postcolumn iron(III) salicylate reagent was prepared at 250 µM in aqueous formate buffer, delivered using a syringe pump at a flow rate of 0.5 mL/min. The proposed method was validated as per the guidelines of the International Conference on Harmonization Q2(R1) and was found linear over the range 40–120 µg/mL (r = 0.9995) with a limit of detection of 3.19 µg/mL. Compared to currently reported methods, the proposed method is considerably simpler, faster, cheaper, and adequately sensitive and makes use of the most popular LC detectors.


Bisphosphonates Non-chromophoric drugs Highly polar compounds High-performance liquid chromatography Reversed phase 



There was no funding submitted for this project.

Compliance with Ethical Standards

Conflict of interest

The authors declared no conflict of interests.

Consent for publication

All the authors gave their consent for the publication of this article.

Ethics approval

The experiments were conducted according to the rules of the Ethical Committee of the Faculty of Pharmacy, Tanta University, Egypt. No studies with human participants or animals were performed by any of the authors in this work.

Supplementary material

41664_2019_115_MOESM1_ESM.docx (78 kb)
Supplementary material 1 (DOCX 77 kb)


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Copyright information

© The Nonferrous Metals Society of China 2019

Authors and Affiliations

  1. 1.Department of Pharmaceutical Analytical Chemistry, Faculty of PharmacyTanta UniversityTantaEgypt
  2. 2.Pharmaceutical Services Center, Faculty of PharmacyTanta UniversityTantaEgypt
  3. 3.Department of Pharmaceutical Analytical Chemistry, Faculty of PharmacyKafrelsheikh UniversityKafrelsheikhEgypt

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