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建立了同时检测霉千张中黄曲霉毒素等13种真菌毒素的超高效液相色谱-串联质谱(UHPLC-MS/MS)检测方法。样品经乙腈-水(50:50,V/V)提取,Mycospin 400净化。采用ZORBAX Eclipse Plus C_(18)色谱柱(100 mm×2.1,1.8μm)作为分析柱,以10 mmol/L乙酸铵-0.5%乙酸-水和10 mmol/L乙酸铵-0.5%乙酸-乙腈作为流动相进行梯度洗脱,电喷雾正、负离子(ESI+,ESI-)多反应模式监测。评估了每种真菌毒素在霉千张样品中的基质效应,采用同位素内标法进行定量分析。结果表明,13种真菌毒素在1.0~500μg/kg范围呈良好线性,所得R2均大于0.999。样品在高、中、低3个浓度加标水平下的平均回收率为69.8%~118.4%,相对标准偏差(RSD)为1.4%~15%。针对不同真菌毒素,方法的定量限为1.0~30μg/kg。
An ultra-performance liquid chromatography-tandem mass spectrometry (UHPLC-MS / MS) method was developed for the simultaneous determination of 13 mycotoxins such as aflatoxins in Mechuensis. Samples were extracted with acetonitrile-water (50:50, V / V) and Mycospin 400 was purified. A ZORBAX Eclipse Plus C_ (18) column (100 mm × 2.1, 1.8 μm) was used as the analytical column, with 10 mmol / L ammonium acetate-0.5% acetic acid-water and 10 mmol / L ammonium acetate-0.5% acetic acid- Mobile phase gradient elution, electrospray positive and negative ion (ESI +, ESI-) multi-reaction mode monitoring. Matrix effects of each mycotoxin in thousands of samples were evaluated and quantitative analysis was performed using isotope internal standard method. The results showed that 13 kinds of mycotoxins showed a good linearity in the range of 1.0-500 μg / kg, and the obtained R2 values were all greater than 0.999. The average recoveries of the samples were 69.8% -118.4% with RSDs of 1.4% -15% at the three spiked levels of high, medium and low concentrations. For different mycotoxins, the limit of quantification is 1.0 ~ 30μg / kg.