ABSTRACT
A new, simple, and sensitive method was developed for extraction of ochratoxin A (OTA) in beer combined with HPLC-fluorescence detector. Samples were extracted by stir bar sorptive extraction (SBSE) followed by liquid desorption using commercially available Twister EG-Silicone. The main parameters influencing SBSE, including phase ratio, extraction time, stirring speed, ionic strength, organic modifier, pH, temperature, desorption mode, desorption solvent, and desorption time were optimized. Under the optimal conditions, assay was performed on 4 mL of samples acidified at pH 1.5. The samples were extracted for 180 min at a stirring speed of 800 rpm followed by desorption of analyte using 1 mL methanol under sonication for 45 min. The extract was evaporated at 50 degrees C under a gentle nitrogen stream, then redissolved in 200 microL of methanol-water (50 + 50, v/v). After each use, the stir bar was cleaned by sonication in methanol for 30 min three times. The method provided good linearity of the calibration curve with coefficients of determination greater than 0.999. Recoveries of OTA were greater than 83% with RSD lower than 10%, and LOD of OTA in beer was 0.64 ng/L. This method was applied to determine OTA in 19 beer samples. OTA was detected in 12 samples (63%) in the range of 0.01-0.27 ng/mL.
Subject(s)
Beer/analysis , Chemistry Techniques, Analytical , Ochratoxins/analysisABSTRACT
Fast liquid chromatography coupled to triple-quadrupole tandem mass spectrometry was employed for the determination of six UV filters in seawater. The separation of the analytes was achieved in less than 5 min; polarity switching was used as four of the analytes were ionized in positive mode and the remaining two in negative mode. Two ionization sources were employed and compared: atmospheric pressure chemical ionization (APCI) gave better results than electrospray ionization (ESI) for all analytes, with higher reproducibility and lower detection limits. Therefore APCI was chosen for the determination of the analytes in seawater samples using stir bar sorptive extraction-liquid desorption (SBSE-LD). Quantitative analysis was performed in multiple reaction monitoring (MRM) mode; fragmentation pathways of the analytes with regard to the formation of the MRM ions were also proposed. For the analysis of seawater samples, calibration curves were drawn using SBSE in spiked seawater. All figures of merit of the method were satisfactory; limits of detection were particularly low for the four analytes ionized in positive mode, being in the range 8-31 ng/L. The method was applied to the determination of the six UV filters in seawater samples from Liguria, Italy. Only benzophenone-3 (BP-3) and ethylhexyl methoxycinnamate (EHMC) were measured in the analyzed samples; some of the remaining analytes were also detected but always below the limit of quantitation.
