Abstract
The purpose of the present research was to conduct stress degradation studies on the olopatadine hydrochloride, an antiallergic drug, using the hydrophilic interaction liquid chromatography (HILIC). HILIC requires the utilization of polar and moderately polar stationary phases and aqueous-organic mobile phase usually containing more than 70% of organic solvent. In this study, olopatadine hydrochloride was subjected to acid and base hydrolysis, oxidation and termolytic degradation in order to estimate its stability under different stress conditions recommended by ICHQ1A (R2) guideline. Degree of degradation was followed by HILIC method. The chromatographic conditions were: column Betasil Cyano (100 mm ? 4.6 mm, 5 mm particle size), mobile phase consisted of acetonitrile and ammonium acetate 5 mM (pH adjusted to 4.50) in ratio 85:15 V/V, flow rate was 1 mL min-1, column temperature was set at 30?C and detection was performed at 257 nm. Results obtained for stress studies indicated that olopatadine hydrochloride underwent transformation under acidic and oxidative (30% w/v hydrogen peroxyde) conditions showing high degree of degradation. Furthermore, it was found that olopatadine hydrochloride is relatively stable when exposed to thermal (60?C) and basic (1 M NaOH) conditions. Therewith, kinetics of degradation reaction was determined with an aim to define the corresponding reaction rate constants and half-lives. Firstly, the order of the reaction was evaluated experimentally using the integral method. Based on the calculated values of the correlation coefficients, it was shown that the acidic, basic and oxidative degradation are the second-order reaction. High stability under basic conditions was achieved on the basis of the great degradation half-life values. Also, it has been verified that acidic degradation is the fastest reaction.
Highlights
Olopatadine hydrochloride was subjected to acid and base hydrolysis, oxidation and thermolytic degradation in order to estimate its stability under different stress conditions recommended by ICHQ1A (R2) guideline
The chromatographic conditions were: column Betasil Cyano (100 mm×4.6 mm, 5 μm particle size), mobile phase consisted of acetonitrile and ammonium acetate 5 mM in ratio 85:15 V/V, flow rate was 1 mL min–1, column temperature was set at 30 °C and detection was performed at 257 nm
Results obtained for stress studies indicated that olopatadine hydrochloride underwent transformation under acidic and oxidative (30% hydrogen peroxyde) conditions showing high degree of degradation
Summary
Studije forsirane degradacije ili stres studije sprovode se u cilju ispitivanja osnovne hemijske stabilnosti aktivne farmaceutske supstance i farmaceutskog doziranog oblika [1]. Cilj ovog rada je izvođenje studija forsirane degradacije na olopatadin-hidrohloridu i praćenje nastalih proizvoda degradacije metodom tečne hromatografije hidrofilnih interakcija Olopatadin-hidrohlorid je oficinalan u USP/NF farmakopeji, koja za određivanje aktivne farmaceutske supstance i srodnih supstanci propisuje metodu reversno-fazne tečne hromatografije (eng. Reverse Phase High Performance Liquid Chromatography – RP-HPLC) [16]. Kvantitativna analiza aktivne supstance u formulaciji i studije forsirane degradacije izvedene su i primenom RP-HPLC metode za praćenje stabilnosti [22]. Pregled literature pokazao je da stabilnost olopatadin-hidrohlorida nije još uvek dovoljno proučena, kao i da u dosadašnjoj literaturi nije opisana primena HILIC metode za praćenje stepena degradacije ispitivanog jedinjenja pod stres uslovima
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