Abstract
Solid bar microextraction (SBME), followed by liquid chromatography with fluorescence detection (HPLC-FLD), for the quantification of ochratoxin A in wheat and maize was developed. Ground wheat and maize grains were extracted with acetonitrile-water-acetic acid (79:20:1, v/v/v), followed by defatting with cyclohexane, and subjected to SBME-LC-FLD analysis. SBME devices were constructed by packing 2 mg sorbent (C18) into porous polypropylene micro-tubes (2.5 cm length, 600 μm i.d., and 0.2 μm pore size). SBME devices were conditioned with methanol and placed into 5 mL stirred sample solutions for 70 min. After extraction, OTA was desorbed into 200 μL of methanol for 15 min, the solution was removed in vacuum, the residue was dissolved in 50 μL of methanol-water (1:1, v/v) and ochratoxin A content was determined by HPLC-FLD. Under optimized extraction conditions, the limit of detection of 0.9 μg·kg−1 and 2.5 μg·kg−1 and the precision of 3.4% and 5.0% over a concentration range of 1 to 100 μg·kg−1 in wheat and maize flour, respectively, were obtained.
Highlights
Mycotoxin ochratoxin A (OTA) is produced by numerous Penicillium and Aspergillus species such as Penicillium verrucosum, Penicillium nordicum, Aspegillus ochraceus, and Aspergillus carbonariusm, while new producers are continuously being discovered [1]
We investigated the application of Solid bar microextraction (SBME) combined with HPLC-FLD to determine OTA
The following solid phase microextraction (SPME) parameters were optimized for maximum OTA recovery: type of sorbent, number of SBME devices used, sample pH, extraction time, stirring speed, and desorption conditions
Summary
Mycotoxin ochratoxin A (OTA) is produced by numerous Penicillium and Aspergillus species such as Penicillium verrucosum, Penicillium nordicum, Aspegillus ochraceus, and Aspergillus carbonariusm, while new producers are continuously being discovered [1]. Interesting new developments include the use of ionic liquids as extraction solvents in LLE [18], cleanup of OTA by coacervation of reverse micelles [23], and liquid-liquid microextraction in porous hollow fibers [24]. Both SPE (except for the immunoaffinity columns) and LLE in a traditional setup require multistep protocols that are time-consuming and use large volumes of organic solvents; see [25] for a summary of the drawbacks. Since cereal grains are the main source of OTA exposure [3], and maize is a staple grain in many countries, we have chosen wheat and maize as matrices for which the performance parameters of the method were determined
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