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目的建立酸枣仁中赭曲霉毒素A的LC-MS/MS测定方法,着重于方法的提取与净化、质谱参数的分析等过程。方法以酸枣仁为研究基质,采用改良Qu ECh ERS法,均质样品经水浸泡后,加入10%甲酸-乙腈溶液进行提取,同时加入莠去津作为内标;乙腈溶液经分散固相萃取技术净化后,用高效液相色谱-串联质谱法进行分析测定。结果赭曲霉毒素A在0.05 ng/ml~5 ng/ml时进样量与峰面积呈良好的线性关系,加样回收率为72.11%~85.00%。方法的重复性及稳定性均良好;检出限为0.1μg/kg。改良Qu ECh ERS法既省时又经济有效。结论本法简便快速、灵敏度高、结果准确,可用于酸枣仁中赭曲霉毒素A的测定分析。
OBJECTIVE To establish a method for the determination of ochratoxin A in Semen Ziziphi spinosa L., with emphasis on the extraction and purification of the method and the analysis of mass spectral parameters. The method was based on the improved Qu ECh ERS method. After homogenized samples were immersed in water, 10% formic acid-acetonitrile solution was added for extraction and atrazine was added as internal standard. The acetonitrile solution was separated by solid-phase extraction After purification, analysis was performed by high performance liquid chromatography-tandem mass spectrometry. Results There was a good linear relationship between the injection volume of ochratoxin A and the peak area at the concentration of 0.05 ng / ml ~ 5 ng / ml. The recoveries were 72.11% ~ 85.00%. The repeatability and stability of the method were good. The detection limit was 0.1 μg / kg. Improved Qu ECh ERS method is time-saving and cost-effective. Conclusion This method is simple, rapid, sensitive and accurate. It can be used to determine ochratoxin A in wild jujube.