Extraction and determination of fluoroquinolones in milk samples using solid phase extraction and liquid chromatography - tandem mass spectrometry.
Author
Al-Sharjiyah, Nada Ahmed Hamdoon.
Publisher
Sultan Qaboos University.
English abstract
A solid phase extraction (SPE) and high-performance liquid Chromatography coupled
with tandem mass spectrometry (HPLC-MS/MS) method was developed and validated
for qualitative and quantitative determination of fluoroquinolone (FQ) compounds in
milk samples. The FQ compounds were: ofloxacin, norfloxacin and ciprofloxacin.
Extraction of FQs was carried out using two types of sorbents: magnetic nano particles
(MNP) and styrene divinyl benzene co-polymer. Two types of MNP were used
including: graphene magnetite (GM) and graphene oxide magnetite (GOM). Results
showed that styrene divinyl benzene co-polymer gives high recoveries (85-100%) with
optimum condition for the extraction of the three analytes using elution solvent 90:10 %
of ACN: MeOH. The optimum mobile phase used consist of solvent A 0.1% formic acid
and methanol as solvent B (75:25). Moreover, MS/MS conditions were optimized in
positive modes. Multiple reaction-monitoring modes (MRM) were used to determined
precursor ion and product ions of the FQs compounds. The developed method was
validated. The linear regression (R2
) ranged between 0.996 and 0.997 while the limit of
detection (LOD) was between 0.0032 and 0.016 ng mL-1
. Finally, milk samples
purchased from the local market were analyzed and results showed low traces of FQs
compounds are presents in these samples.
Identifier
Al-Sharjiyah, Nada Ahmed Hamdoon (2020). Extraction and determination of fluoroquinolones in milk samples using solid phase extraction and liquid chromatography - tandem mass spectrometry (Master thesis, Sultan Qaboos University, Muscat, Oman).
