Determination of aflatoxins in rice from Penang, Malaysia by dispersive liquid–liquid micro-extraction and LC–MS/MS

Abstract

Rice is one of the crops cultivated in Malaysia, and it is the main diet for most of the population. In this study, dispersive liquid–liquid micro-extraction (DLLME) and liquid chromatography–tandem mass spectrometry (LC–MS/MS) were used to develop, optimise and validate a reliable, easy-to-use and quick approach to detect aflatoxin B1 (AFB1), aflatoxin B2 (AFB2), aflatoxin G1 (AFG1) and aflatoxin G2 (AFG2). The extraction recoveries in DLLME were enhanced by the addition of 5% salt, utilising chloroform as the extraction solvent and acetonitrile as the dispersive solvent. The DLLME parameters – the extraction solvent volume, salt concentration and dispersive solvent volume were optimised with Box–Behnken design (BBD) and response surface methodology (RSM). Under optimised experimental conditions, excellent linearity was obtained with a limit of detection (LOD) ranging from 0.125 to 0.25 ng g⁻¹, a limit of quantitation (LOQ) ranging from 0.25 to 0.3 ng g⁻¹ and a correlation value (R²) of 0.990. The matrix effects were between −11.1% and 19.9%, and recoveries ranged from 87.4% to 117.3%. The optimised and validated method was used effectively to assess aflatoxins contamination in 20 commercial rice samples collected from local supermarkets in Penang, Malaysia. AFB1 was detected at 0.41–0.43 ng g⁻¹ in two rice samples, below the regulatory limit.

Keywords:

• Aflatoxins
• rice
• response surface methodology
• Box–Behnken design

Author contributions

Conceptualization, S.S.A. and I.M.N; Methodology, S.S.A. and I.M.N; Validation, S.S.A., B.N.H, I.N.S and A.G.Z; Investigation, S.S.A., B.N.H, I.N.S and A.G.Z; Resources, S.S.A and I.M.N; Writing—Original Draft Preparation, S.S.A.; Writing—Review and Editing, S.S.A and I.M.N.; and Supervision, I.M.N.

Disclosure statement

There are no conflicts to declare.

Additional information

Funding

The study was supported by Universiti Sains Malaysia through the Short-Term Grant Scheme [304.CABR.6315570].