Razvoj i validacija LC metode za vrednovanje procesa čišćenja opreme nakon proizvodnje Betazon kreme i Betazon masti

master's thesis

• Title (english): Development and validation of LC method for evaluation of the equipment cleaning process after production of Betazon cream and Betazon ointment
• Author: Ivan Sušanj
• 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: 2018-07-11, Croatia
• Scientific / art field, discipline and subdiscipline: BIOMEDICINE AND HEALTHCARE; Pharmacy; Pharmacy

Abstract

Betametazondipropionat aktivna je komponenta topičke formulacije čija je proizvodnja izabrana
kao najsloženiji slučaj procesnih uvjeta prilikom izrade polučvrstih oblika. Razvijena je i
validirana UPLC metoda za određivanje ostataka betametazondipropionata nakon proizvodnje
Betazon® kreme i Betazon® masti. Tijekom razvoja definirani su sljedeći kromatografski uvjeti:
protok od 0,75 mL/min, valna duljina detekcije od 240 nm, kolona Zorbax Extend-C18 100 x 3,0
mm, 1,8μm temperirana na 25°C, mobilna faza acetonitril za kromatografiju R : voda za
kromatografiju R = 60 : 40 (V/V%), volumen injektiranja od 40μL, temperatura injektora 20°C i
vrijeme eluacije 8 minuta.
Validacijska studija provedena je samo na materijalu inoks zbog odluke o nabavi jednonamjenskih
silikonskih cijevi u proizvodnji Betazon® kreme i Betazon® masti. Metoda je uspješno validirana
kroz parametre: selektivnost, linearnost, radno područje, točnost, limit detekcije i limit
kvantifikacije. Ispitana je i stabilnost poredbene otopine, cijepljenog ispirka, cijepljenog brisa i
„suhog“ cijepljenog brisa te je određen faktor iskoristivosti za bris i ispirak. Limit kvantifikacije
metode iznosi 0,04 μg/mL, a radno područje je u rasponu od 0,04-0,54 μg/mL
betametazondipropionata.

Abstract (english)

Betamethasone dipropionate is an active pharmaceutical ingredient in topical formulation wich
production has been chosen as the worst case scenario in production of semi-solid products. UPLC
method has been developed and validated for determining the residues of betamethasone
dipropionate after production of Betazon ® cream and Betazon® ointment. During development,
next chromatographic conditions have been defined: flow 0,75 mL/min, detection wavelength 240
nm, column Zorbax Extend-C18 100 x 3,0 mm, 1,8 μm tempered at 25°C, mobile phase containing
acetonitrile for chromatography R : water for chromatography R = 60 : 40 (V/V%), injecting
volume 40μL, injector temperature 20°C and run time 8 minutes.
Validation study has been conducted for inox material only due to decision of using dedicated
silicon plumbs in production of Betazon ® cream and Betazon® ointment. Method has been
successfully validated through next parameters: selectivity, linearity, range, accuracy, limit of
detection and limit of quantitation. Stability of reference solution, spiked eluate, spiked swab and
„dry“ spiked swab has also been studied and recovery factors have been determined for both eluate
and swab. Method´s limit of quantitation is 0,04 μg/mL and range is in span from 0,04 to 0,54
μg/mL of betamethasone dipropionate.

• Keywords: betametazondipropionat; UPLC; vrednovanje procesa čišćenja; validacija analitičke metode
• Keywords (english): betamethasone dipropionate; UPLC; cleaning validation; validation of analytical procedure
• Language: croatian
• URN:NBN: urn:nbn:hr:163:147326
• 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: 2018-12-03 13:07:37