Određivanje fosfata ionskom kromatografijom u različitim ljekovitim tekućim oblicima uz ispitivanje razvojno-validacijskih parametara

master's thesis

• Title (english): Development and validation of method for phosphate determination by ion chromatography in liquid pharmaceutical products
• Author: Maria Grbavac
• Mentor: Biljana Nigović (mentor)
• Committee member: Biljana Nigović (predsjednik povjerenstva)
• Committee member: Ana Mornar Turk (član povjerenstva)
• Committee member: Danijela Štanfel (član povjerenstva)
• Granter: University of Zagreb; Faculty of Pharmacy and Biochemistry; (Department of pharmaceutical analysis); Zagreb
• Defense date and country: 2021-03-19, Croatia
• Scientific / art field, discipline and subdiscipline: BIOMEDICINE AND HEALTHCARE; Pharmacy; Pharmacy

Abstract

Sterilni farmaceutski proizvodi u tekućem obliku za primjenu u oftalmologiji i otorinolaringologiji su strateški fokus kompanije JGL d.d., stoga je svrha rada bila razviti i validirati metodu koja će moći pouzdano odrediti sadržaj fosfata takvim proizvodima te koja bi trebala biti potpora procesu razvoja formulacije.
Metoda je razvijena na sustavu za ionsku kromatografiju Dionex ICS-5000+ sa sljedećim komponentama: Dionex ICS-5000+ DP, Dionex ICS-5000+ EG, Dionex ICS-5000+ DC i Dionex AS-AP. Definirani su sljedeći radni uvjeti metode: volumen injektiranja 25 μL, brzina protoka mobilne faze 0,6 mL/min, sastav mobilne faze 4 mM K2CO3/0,5 mM KHCO3, temperatura kolone 30°C, pretkolona Dionex IonPac AG14A, kolona Dionex IonPac AS14A (3x150 mm) i trajanje metode 16 min. Primijenjena je konduktometrijska metoda detekcije uz supresiju mobilne faze.
Metoda je u radnom području 10-50 μg/mL fosfata zadovoljila zahtjeve za sljedeće parametre validacije: selektivnost, linearnost, točnost, preciznost sustava, preciznost metode, središnja preciznost i otpornost na promjene uvjeta metode. Ispitan je i utjecaj filtriranja na koncentraciju fosfata u uzorcima za analizu, te stabilnost otopina standarda, koncentracijskog niza i otopina uzoraka.

Abstract (english)

Sterile liquid pharmaceutical products for use in ophthalmology and otorhinolaryngology are the strategic focus of JGL d.d. Therefore, the purpose of this work was to develop and validate a reliable method for determination of phosphate content in such products and support the formulation development process.
The method was developed on the Dionex ICS-5000+ ion chromatography system with the following components: Dionex ICS-5000+ DP, Dionex ICS-5000+ EG, Dionex ICS-5000+ DC and Dionex AS-AP. Defined operating conditions of the method are: injection volume 25 μL, mobile phase flow rate 0,6 mL/min, mobile phase composition 4 mM K2CO3/0,5 mM KHCO3, column temperature 30°C, pre-column Dionex IonPac AG14A, column Dionex IonPac AS14A (3x150 mm) and duration 16 min. Conductometric detection with mobile phase suppression was applied as a method of detection.
The method met the requirements for the following validation parameters: selectivity, linearity, accuracy, repeatability, precision, intermediate precision and robustness within the working range of 10-50 μg/mL phosphate concentration. The impact of filtering on phosphate concentration in final analysis samples, the stability of calibration solutions and sample solutions were also assessed.

• Keywords: ionska kromatografija; fosfati; tekući oblici; razvoj metode; validacija metode
• Keywords (english): ion chromatography; phosphates; liquid pharmaceutical products; method development; method validation
• Language: croatian
• URN:NBN: urn:nbn:hr:163:331547
• Study programme: Title: Pharmacy; Study programme type: university; Study level: integrated undergraduate and graduate; Academic / professional title: magistar/magistra farmacije (magistar/magistra farmacije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access
• Created on: 2021-11-15 13:34:45