Determination of 5 Mycotoxins in Quzhou Aurantii Fructus by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Composite Immunoaffinity Column Purification
Determination of 5 Mycotoxins in Quzhou Aurantii Fructus by Ultra-High Performance Liquid Chromatography-Tandem Mass Spectrometry with Composite Immunoaffinity Column Purification
The method mentioned by the title was proposed to determine aflatoxin B1,B2,G1,G2,and ochratoxin A in Quzhou Aurantii Fructus samples.After ultrasonic extraction on the sample in the mixed solution composed of acetonitrile,water and acetic acid at volume ratio of 79∶20∶1,the extract was centrifuged.The supernatant was diluted by phosphate buffer solution(pH 7.0),purified with a composite immunoaffinity column,and filtered.The targets in the filtrate was separated on the XDB C18 chromatographic column using mixed solutions composed of methanol-5 mmol·L-1 ammonium acetate mixed solution(volume ratio of 1∶9)and methanol-5 mmol·L-1 ammonium acetate mixed solution(volume ratio of 9∶1)at different volume ratios,detected by the ESI+and MRM modes,and quantified by the isotope internal standard method.It was shown that linear relationships between values of the mass concentration ratio and corresponding peak area ratio of the 5 mycotoxins to their isotope internal standards were kept in definite ranges,with detection limits in the range of 0.05-0.20 μg·kg-1.Recoveries of the 5 mycotoxins in negative samples at three spiked concentration levels ranged from 82.7%to 97.3%,and RSDs(n=6)of the determined values were in the range of 5.2%-12%.
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