validation | Acta Medica Marisiensis

Development and Validation of an UV-Spectrophotometric Method for the Assay of Strontium Ranelate and HPLC Stability Testing from Bulk and Pharmaceutical Dosage Form

Béla Kovács¹, Réka Molnár², Előd Ernő Nagy³, Éva Katalin Kelemen⁴, Blanka Székely-Szentmiklósi³, István Székely-Szentmiklósi^4,5, Boglárka Kovács-Deák⁶, Árpád Gyéresi⁷

1. University of Medicine, Pharmacy, Sciences and Technology of Târgu Mureș, Romania
2. First Department of Internal Medicine, Faculty of Medicine, University of Szeged, Hungary
3. Department of Biochemistry and Environmental Chemistry, Faculty of Pharmacy, University of Medicine, Pharmacy, Sciences and Technology of Târgu Mureș, Romania
4. Gedeon Richter, Târgu Mureș, Romania
5. Department of Pharmaceutical Industry and Management, Faculty of Pharmacy, University of Medicine, Pharmacy, Sciences and Technology of Târgu Mureș, Romania
6. Salvator Pharmacy, Târgu Mureș, Romania
7. Department of Pharmaceutical Chemistry, Faculty of Pharmacy, University of Medicine, Pharmacy, Sciences and Technology of Târgu Mureș, Romania

DOI: 10.2478/amma-2019-0014

Objective: The present work offers a fast, reliable and easy UV spectrophotometric method for the assay of strontium ranelate from bulk samples and pharmaceutical dosage form.
Methods: The proposed method uses 0.1% V/V trichloroacetic acid as dissolution medium for spectrophotometric analysis, by signal detection at 321 nm. The method was validated according to the currently in-force international guidelines for linearity, accuracy, precision, robustness, limit of detection and quantification.
Results: The method was found to be linear in the range of 5-100 µg mL-1 (R2 > 0.999). Method accuracy was found in-between 98.87-100.41%, showing good linear correlation as well (R2 = 0.9997). The concentrations for limit of detection and limit of quantitation were found 1.13 µg mL-1 and 3.77 µg mL-1, resp. The proposed method showed good intra- and interday precision, with low RSD values of 0.53-1.24% and 1.11%, resp.
Conclusions: Stability studies performed by both HPLC and UV spectrophotometric methods revealed that the active substance is highly susceptible to acidic hydrolysis, oxidation and exposure to high temperature.

Is the Doppler Ultrasound Score More Reliable than the Grey Scale Ultrasound Score in Assessing the Rheumatoid Arthritis Patient’s Joints?

Copotoiu Monica¹, Georgescu Lia¹, Poór G², Copotoiu Ruxandra³

1 Department of Rheumatology, University of Medicine and Pharmacy, Tîrgu Mureș, Romania
2 1st Department of Rheumatology, National Institute of Rheumatology and Physiotherapy, Budapest, Hungary
3 Department of Anaesthesia and Intensive Care, University of Medicine and Pharmacy, Tîrgu Mureș, Romania

Background: Rheumatoid arthritis (RA) is a complex disease with multiple faces, one of them being its activity. At the moment, there are multiple-choice tools to assess the activity of the disease, no one gaining the complete status of “gold standard”. In the evaluation of the disease activity biological and non-biological methods are used and interposed. The methods are more or less subjective, thus the validation of measurements in RA is highly relevant.
Objective: The main objective of the study was to evaluate the reliability of the Doppler Ultrasound score versus the Grey scale ultrasound score in the assessment of the disease activity in rheumatoid arthritis patients.
Methods: A number of 66 patients diagnosed with rheumatoid arthritis were assessed with the B-mode and consequently Colour Doppler ultrasound score system. The joints examined were the second and the third metacarpal (MCP) and proximal interphalangeal joints (PIP) on the dorsal and ventral side. Two thousand twelve images were stored and evaluated on both scales. Data were analysed with GraphPad Prism 5.0. In order to assess the validity of the ultrasound methods used in the study as non-biological markers for the activity of rheumatoid arthritis Pearson correlation, Bland-Altman method and linear regression were used.
Results: A positive correlation was found when analyzed the two methods of assessment of the disease activity in rheumatoid arthritis. A single mismatch was found (Pearson correlation and linear regression) at the level of the second metacarpal on the ventral and right side when compared the Doppler ultrasound versus the Grey scale score, but we presumed that this is due to the particularity of the individual outcome. The Bland-Altman method showed that the Grey scale of quantification overrated the scores versus the Color Doppler Ultrasound scale.
Conclusions: The semi-quantitative Color Doppler method which assesses the intra-joint activity in rheumatoid arthritis patients was validated in our research to be further used. Even though none of the statistic methods used for validating the Doppler score in our study showed significant statistic differences between them, it is for the best to apply all of them for validating any intended method to be used in any study.