【摘要】 目的建立超高效液相色谱-串联三重四级杆质谱(UPLC-MS/MS)测定面包、馒头和饼干等粮食制品中4种真菌毒素的方法。方法样品用乙腈-水(84∶16,V/V)超声提取,经QuEChERS方法净化,采用BDS HYPERSIL C18色谱柱(4.6 mm×100 mm,2.4μm)进行分离,以甲醇-乙酸铵缓冲液为流动相梯度洗脱,流速为300μl/min,在电喷雾负离子化模式(ESI-)和多反应监测模式(MRM)下进行检测,采用基质外标法定量。并对方法的检出限、定量限、准确度和精密度进行评价,用建立的方法对60份市售粮食制品中的4种真菌毒素进行检测。结果在优化条件下,4种真菌毒素在各自的线性范围内线性关系良好,相关系数(r)均不低于0.999,回收率在81.8%~98.2%之间,相对标准偏差在5.6%~9.3%之间。60份市售粮食制品中均检出脱氧雪腐镰刀菌烯醇,含量为15.2~960μg/kg,其余3种真菌毒素均未检出。结论该方法与国家标准方法和国家食品安全风险监测方法比较,具有操作简单、成本低的优点,且速度快、灵敏度高、重现性好,完善了我国食品安全风险监测的方法。更多还原

【Abstract】 Objective A high performance liquid chromatography coupled to mass spectrometry( UPLC-MS/MS) method was developed for the determination of four mycotoxins in grain products such as bread,steamed bun and biscuit. Methods Samples were extracted with acetonitrile-water( 84 ∶ 16, V/V), then was purified by QuEChERS approach. UPLC separation was achieved by using BDS HYPERSIL C18( 4. 6 mm × 100 mm,2. 4 μm) chromatographic column by gradient elution at a flow rate of 300 μl/min with methanol and acetate buffer as the mobile phase. The detection was carried out by negative electrospray ionization( ESI-) mass spectrometry in multiple reaction monitoring mode( MRM). Matrix-matched calibration was used for the quantification. The limits of detection,quantification,accuracy and precision of the method were evaluated. The method was used for detecting four mycotoxins in 60 different grains from the market. Results Under optimized condition,four mycotoxins had good linear relationships in the certain correlation ranges with the correlation coefficients all above 0. 999. The average recoveries of 4 mycotoxins at three spiked levels ranged from 81. 8% to 98. 2%with relative standard deviations of 5. 6%-9. 3%. Four mycotoxins were detected in the 60 market samples. Deoxynivalenol( DON) was detected in all samples with the concentrations of 15. 2-960 μg/kg,the other 3 mycotoxins were not detected.Conclusion The method was more simple and lower cost than the national standard method and the national food safety risk monitoring method,with fast speed,high sensitivity and good reproducibility,which improve the national food safety risk monitoring method.更多还原