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目的:采用超高压液相色谱-四极杆质谱联用技术UPLC-MS/MS,同时测定玉米中的赭曲霉素A等10种霉菌毒素。方法:样品用84/16的乙腈/水混合液匀浆提取3 min,经一种创新型的自制混合固相萃取柱纯化后经Acquity UH-PLC HSS T3柱(100 mm×2.1 mm,1.7μm particle size)分离,10 min内10种霉菌毒素完全分离。结果:采用13C-DON同位素内标法定量,MON 10~5000μg/kg,OTA 0.2~50μg/kg,OTB 0.2~50μg/kg,NIV 2~500μg/kg,ZON 5~500μg/kg,DON2~500μg/kg,15-ADON2~500μg/kg,3-ADON2~500μg/kg,ZAN 2~500μg/kg的浓度范围内呈良好的线性关系,r≥0.999。相对加样平均回收率为:75.8%~106.5%,RSD:1.7%~9.6%;LOQ在0.09~8.48μg/kg,满足欧盟限量标准。结论:该方法具有预处理简单、检测速度快、灵敏度高的优点,可适用于玉米样品中霉菌毒素的确认和准确定量检测,可满足各国对霉菌毒素的最低检出要求。运用建立的方法对各地的69份玉米产品进行含量测定,玉米样品中普遍存在霉菌毒素的污染。
OBJECTIVE: To determine the content of 10 mycotoxins including ochratoxin A in maize by UPLC-MS / MS with UHPLC-quadrupole mass spectrometry. Methods: Samples were homogenized with a mixture of acetonitrile and water (84/16) for 3 min and purified by an innovative home-made mixed SPE column. The samples were separated on an Acquity UH-PLC HSS T3 column (100 mm × 2.1 mm, 1.7 μm particle size, 10 mycotoxins were completely separated within 10 min. Results: Quantities of MON 10 ~ 5000μg / kg, OTA 0.2 ~ 50μg / kg, OTB 0.2 ~ 50μg / kg, NIV 2 ~ 500μg / kg, ZON 5 ~ 500μg / kg and DON2 ~ 500μg were quantified by13C-DON isotope internal standard method. kg / kg, 15-ADON2-500μg / kg, 3-ADON2-500μg / kg and ZAN2-500μg / kg, with a linear relationship of r≥0.999. The relative average recoveries were 75.8% -106.5%, RSD 1.7% -9.6%, and LOQ 0.09-8.48μg / kg, meeting the EU limits. Conclusion: The method has the advantages of simple pretreatment, fast detection and high sensitivity. It can be used to confirm and accurately detect mycotoxins in maize samples and meet the minimum detection requirements of mycotoxins in various countries. The established method was used to determine the contents of 69 corn products in different parts of the country. The contamination of mycotoxins was widespread in corn samples.