In-syringe dispersive micro-solid phase extraction method for the HPLC-fluorescence determination of aflatoxins in milk
2022
Shuib, Nor Shifa | Saad, Bahruddin
The simultaneous determination of aflatoxins (B₁, B₂, M₁ and M₂) in milk using a new sample pretreatment technique, the in-syringe dispersive micro-solid phase extraction (ISDμSPE), coupled with high performance liquid chromatography with fluorescence detection is described. The separation of the aflatoxins were performed using C18 Hypersil gold (250 mm × 4.6 mm, 5 μm) column at 40 °C under gradient elution for 35 min. The excitation and emission wavelengths of the fluorescence detector were at 360 nm and 440 nm, respectively. On-line photo-chemical derivatization was used to enhance the detection of aflatoxin B₁. Several parameters such as type and amount of sorbent, vortex speed, vortex time and elution solvent were evaluated. Limits of detection (LOD) ranged from 0.003 to 0.005 ng mL⁻¹, limits of quantification (LOQ) ranged from 0.01 to 0.02 ng mL⁻¹, recoveries ranged from 73.0 to 109.6%, and relative standard deviations (RSDs) was less than 17.3%. The proposed method was succesfully applied to the analysis of aflatoxins in milk.
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