超高效液相色谱-串联质谱法快速测定稻谷和玉米中伏马毒素

目的 建立了同位素稀释-超高效液相色谱串联质谱法测定稻谷和玉米中伏马毒素。方法 样品加入同位素内标后用50%乙腈水溶液(含1%甲酸)提取,采用ZORBAX Eclipse Plus C18 色谱柱分离,以甲醇-0.1%甲酸水溶液为流动相,梯度洗脱,质谱采用电喷雾电离,负离子模式下,以多反应监测模式(MRM)检测,内标法定量。结果 FB1,FB2和FB3在0.5~100.0μg/L范围内线性关系良好,相关系数均大于0.995,检出限均为1.0μg/kg。在5.0、50.0、500.0μg/kg三个加标浓度水平下,FB1,FB2和FB3的回收率在82.5~107.1%之间,RSD为3.9%~6.2%(n=5)。结论 该方法简单快速,定性定量准确,有效降低了背景干扰,可用于粮食中伏马毒素的检测。

Rapid determination of fumonisins in paddy and maize by ultra performance liquid chromatography-tandem mass spectrometry

Objective To establish a method for the determination of fumonisins in rice and corn by isotopic dilution-ultra performance liquid chromatography tandem mass spectrometry. Methods The samples were extracted with 50% acetonitrile aqueous solution (containing 1% formic acid) after adding isotope internal standard. The samples were separated by ZORBAX Eclipse Plus C18 chromatographic column. Methanol?0.1% formic acid aqueous solution was used as mobile phase, gradient elution was performed, electrospray ionization was used for mass spectrometry, and multiple reaction monitoring mode was used for detection under negative ion mode, and internal standard method was used for quantification. Results The linear relationship of FB1, FB2 and FB3 were good in the range of 0.5?100.0 g/L, the correlation coefficient was greater than 0.995, and the limit of detection was 1.0 g/kg. The recoveries of FB1, FB2 and FB3 were 82.5%?107.1%, and RSDs were 3.9%?6.2% at 5.0, 50.0 and 500.0 g/kg standard concentrations (n=5). Conclusion This method is simple and fast, accurate in qualitative and quantitative analysis, and can effectively reduce background interference. It can be used to detect fumonisins in grain.