Identification of Four Aflatoxins in Fructus amomi using QuEChERS Combined with Ultra-performance Liquid Chromatography-tandem Mass Spectrometry
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Abstract:
A quick, easy, cheap, effective, rugged, and safe solid phase extraction (QuEChERS), in combination with ultra-high performance liquid chromatography–tandem mass spectrometry (UPLC-MS/MS) was established to identify four aflatoxins in Fructus amomi. Optimal experimental conditions were determined by optimizing the QuEChERS pre-treatment technique and the chromatographic and mass spectrometric conditions. The samples were extracted using acetonitrile with 1% formic acid and salted out with anhydrous magnesium sulfate and sodium chloride, then purified using C18, primary secondary amine (PSA), and magnesium sulfate anhydrous. The target analytes were separated on Waters HSS T3 columns (1.8 µm, 2.1 mm×100 mm), eluted by acetonitrile and a 0.1% (V/V) formic acid-5 mmol/L ammonium acetate solution gradient elution was used. Results were detected using MS/MS in positive ion mode under multiple reaction monitoring (MRM); quantification was further conducted using matrix-matched external standard calibrations. Good linearities for the four aflatoxins in the range of 0.20~10.00 μg/L were obtained and the correlation coefficients were >0.998 9. The recoveries were 89.50%~113.12%. The intraday relative standard deviations (Intra-RSDs) and interday relative standard deviations (Inter-RSDs) were 1.31%~6.71% and 1.29%~6.20%, respectively, as determined using spiked samples. The limits of detection and limits of quantification were 0.30~0.60 μg/kg and 1.00~2.00 μg/kg, respectively. The method is simple, rapid, and sensitive. It can be used for the qualitative determination and quantitative analysis of four aflatoxins residues in Fructus amomi.
