Određivanje granice kvantifikacije antibiotika u medu vezanim sustavom tekućinska kromatografija-tandemna spektrometrija masa

master's thesis

• Title (english): Quantification of antibiotics in honey by liquid chromatography tandem mass spectrometry
• Author: Jelena Budimir
• Mentor: Nives Galić (mentor)
• Committee member: Nives Galić (predsjednik povjerenstva)
• Committee member: Biserka Prugovečki (član povjerenstva)
• Committee member: Rosana Ribić (član povjerenstva)
• Committee member: Iva Juranović Cindrić (član povjerenstva)
• Granter: University of Zagreb; Faculty of Science; (Department of Chemistry); Zagreb
• Defense date and country: 2016-02-26, Croatia
• Scientific / art field, discipline and subdiscipline: NATURAL SCIENCES; Chemistry

Abstract

U ovom radu korištena je metoda za kvalitativno i kvantitativno određivanje sulfonamida i kloramfenikola u medu kombiniranom tehnikom tekućinske kromatografije visoke djelotvornosti i spektrometrije masa. Optimizirani su uvjeti za istovremeno izdvajanje sulfonamida i kloramfenikola iz meda ekstrakcijom na čvrstoj fazi, te je optimizacijom uvjeta postignuta niža granica kvantifikacije za sulfonamide koja iznosi 5,0 g/kg. Granica detekcije za kloramfenikol iznosi 0,3 g/kg. Uzorci su ukoncentrirani i pročišćeni ekstrakcijom na čvrstoj fazi (SPE, engl. Solid phase extraction). Daljnja analiza provodila se na temelju podataka o zadržavanju analita na C18 kromatografskoj koloni i podataka dobivenih MS/MS analizom pomoću sustava ABSciex Qtrap 4500. Optimizirani su volumeni otapala za eluiranje kolone za ekstrakciju i pH-vrijednost uzorka. Također je ispitana ponovljivost pripreme uzorka na granicama kvantifikacije, te je izražena relativnim standardnim odstupanjem (RSD). Prinosi metode ekstrakcije za kloramfenikol iznosi 84,62 % i za sulfonamide od 80,80 % do 125,00 %. Kao unutarnji standard tijekom kvantitativne analize spomenutih antibiotika koristio se izotopno obilježeni kloramfenikol, sulfametazin i sulfametoksazol. Metoda se primjenjivala za analizu sulfonamida i kloramfenikola u uzorcima meda prikupljenim sa različitih geografskih lokacija.

Abstract (english)

Quantitative and qualitative method was used for determination of sulfonamides and chloramphenicol in honey by liquid chromatography coupled to mass spectrometry. Conditions were optimized for simultaneous extraction of sulfonamides and chloramphenicol from honey in solid state. Lower detection limit was achieved for sulfonamides (5.0 g/kg). Detection limit for chloramphenicol was 0.3 g/kg. Samples were concentrated and refined by sold phase extraction. Further analysis was conducted by data of analyte retention at the C18 column chromatography and by the MS/MS data obtained with ABSciex Qtrap 4500 system. pH value of sample and the volume of elution solvent were optimized. Repeatability of method was determined and expressed as relative standard deviation (RSD). Extraction recoveries were high with values in the range 84.62 % for chloramphenicol and of 80.80 % to 125.00 % for sulfonamides. Isotopically marked chloramphenicol was used as internal standard for quantitative analysis of antibiotics. Method was applied for determination of antibiotic in honey samples obtained from the various geographical locations.

• Keywords: antibiotici; kloramfenikol; med; sulfonamidi; vezani sustav tekućinska kromatografija tandemna spektrometrija masa (LCMS/MS)
• Keywords (english): antibiotics; chloramphenicol; honey; liquid chromatography coupled to mass spectrometry (LC-MS/MS); sulfonamides
• Language: croatian
• URN:NBN: urn:nbn:hr:217:657624
• Study programme: Title: Graduate Studies in Chemistry; specializations in: Research (scientific-professional) programme; Course: Research (scientific-professional) programme; Study programme type: university; Study level: graduate; Academic / professional title: magistar/magistra kemije (magistar/magistra kemije)
• Type of resource: Text
• File origin: Born digital
• Access conditions: Open access
• Created on: 2017-01-25 14:12:23