同位素稀释-液相色谱/串联质谱法测定粮食产品中多组分真菌毒素

Isotope Dilution and Ultra High Performance Liquid Chromatography/Tandem Mass Spectrometry for Determination of Multi-Mycotoxins in Cereal Products

目的建立快速、简单地检测粮食产品中多组分真菌毒素的超高效液相色谱/串联质谱法。方法粮食产品中的真菌毒素用乙腈-甲酸-水溶液提取后,加水进行稀释并加入同位素内标,经液相色谱分离,三重四级杆串联质谱仪多反应监测模式检测,用同位素内标法进行定量。结果16种真菌毒素在各自的线性范围内线性良好,相关系数均大于0.999,检出限为0.02~2.0μg/kg,定量限为0.05~5.0μg/kg。在低、中、高3个添加水平下,16种真菌毒素的加标回收率为85.3%~114.0%,相对标准偏差为1.0%~5.3%。结论该方法前处理简便、快速,具有很高的准确度和灵敏度高,适用于食品样品中多真菌毒素组分的同时快速检测。

Objective To establish a fast and simple method for determination multi-mycotoxins in cereal products by using ultra high performance liquid chromatography/tandem mass spectrometry.Methods Mycotoxins in samples were extracted by using aeetonitrile/formie acid/water(79∶l∶20,V/V). After diluted by water and added isotope internal standards, mycotoxins were separated by ultra high performance liquid chromatography and measured by multiple reaction monitoring mode of tandem mass spectrometry. Multi-mycotoxins were quantitated by isotope internal standard method.Results The method showed good linearity for 16 mycotoxins in certain correlation ranges. The correlation coefficients were all above 0.999. The detection limit was 0.02-2.0 g/kg,and the quantitative limit was 0.05~5.0 g/kg. Average standard recovery rates of 16 mycotoxins in different kind samples at three spiked levels ranged from 85.3% to 114%, with relative standard deviation varying from 1.0% to 5.3%. Conclusion This method was simple,rapid,sensitive and accurate. It’s suitable for the determination multi-mycotoxins in cereal products.