Lee, Tien Ping
(2013)
Development Of New Analytical Methods
Involving Novel Sorbents And Membranes For The
Determination Of Selected Mycotoxins And
Related Metabolites In Biological
Fluids And Food.
PhD thesis, Universiti Sains Malaysia.
Abstract
This thesis focuses on the development and validation of new sample
preparation methods applied to the determination of mycotoxins and their related
substances. Additionally, a high performance liquid chromatography (HPLC) method
for the determination of sphinganine (Sa) and sphingosine (So) in urine samples by
employing a silica based monolithic column is described. Under the optimized
conditions, separation was achieved using a mixture of methanol:water (93:7, v/v),
column temperature at 30°C, flow rate of 1 mL min-1 and injection volume of 10 μL.
A marked reduction in separation time (less than 6 min) was found compared to
approximately 14 min by using a conventional C18 particle column. Twenty two
urine samples from the healthy donors and seven samples from the liver cancer
patients were analyzed using the method. Molecularly imprinted polymers (MIPs) for
citrinin (CTN) were prepared with 1-hydroxy-2-naphthoic acid (HNA) and 1-
naphthol (NA) as mimic template. Hybrid MIP membrane were next prepared by
embedding the NA-MIP particles into the polyethersulfone scaffold using phase
inversion technique. The resultant membranes were evaluated for the extraction of
CTN and were determined using HPLC with fluorescence detection.
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