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目的建立测定小麦终产品中4种B类单端孢烯霉族类真菌毒素的液质联用同位素内标法。方法馍馍、面包、面条3类样品粉碎混匀后经乙腈-水溶液(84∶16,V/V)提取,Romer Myco Sep 226多功能净化柱净化,Thermo TSQ Quantum Access Max三重四级杆质谱电喷雾负离子源(ESI-),多反应监测(MRM)方式进行检测,同位素内标法定量。结果 4种真菌毒素在5.00μg/L~500μg/L呈良好线性关系(r≥0.999 0),检出限为0.18μg/kg~0.25μg/kg,精密度相对标准偏差为2.46%~10.30%,加标回收率为70.8%~107.6%。结论此方法灵敏度高,线性范围较宽,可满足不同浓度的小麦终产品中4种真菌毒素的同时检测。
Objective To establish a liquid chromatography-mass spectrometry (LC-MS / MS) isotope internal standard method for the determination of four B-type mycotoxins in wheat end products. Methods Three types of 馍 馍, bread and noodle samples were crushed and mixed, extracted with acetonitrile-water solution (84:16, V / V), purified with Romer Myco Sep 226 multifunctional purification column, Thermo TSQ Quantum Access Max triple quadrupole mass spectrometer Spray negative ion source (ESI-), multiple reaction monitoring (MRM) method for detection, isotope internal standard method. Results The linear range of the four mycotoxins was 5.00μg / L ~ 500μg / L (r≥0.999 0), the detection limit was 0.18μg / kg ~ 0.25μg / kg, the relative standard deviations of precision were 2.46% -10.30% , The spiked recoveries ranged from 70.8% to 107.6%. Conclusion This method has high sensitivity and wide linear range and can meet the simultaneous detection of four mycotoxins in different concentrations of wheat end products.