超高效液相色谱-串联质谱法同时测定小麦中的4种限量真菌毒素

Simultaneous determination of 4 limited mycotoxins in wheat by ultra performance liquid chromatography-tandem mass spectrometry

目的建立复合免疫亲和柱净化-超高效液相色谱-串联质谱法同时测定小麦中4种限量真菌毒素的分析方法。方法小麦样品粉碎后,通过80%的乙腈水溶液(V:V)提取后,采用复合免疫亲和柱净化,并利用超高效液相色谱串联质谱的多反应监测模式进行测定分析。色谱柱为ACQUITYUPLCBEHC18柱(100 mm×2.1 mm, 1.7μm),以10 mmol/L乙酸铵(含0.1%甲酸)-甲醇为流动相梯度洗脱,在电喷雾电离模式下正、负离子同时扫描检测,采用外标法定量。结果在8.0 min内可以完成4种真菌毒素的测定,在相应的线性范围内,回归方程的相关系数均超过0.999,3个加标水平下,回收率为82.0%~103.0%,相对标准偏差为5.2%~9.7%。结论该方法快速、准确、高效,适用于小麦及其制品中4种限量真菌毒素的同时测定。

Objective To establish a method for simultaneous determination of 4 limited mycotoxins in wheat by immunoaffinity column purification-ultra performance liquid chromatography-tandem mass spectrometry. Methods Wheat samples were extracted by 80%(V:V) acetonitrile aqueous solution after crushing, purified by combination immunoaffinity column, and determined by multi-reaction monitoring mode of ultra performance liquid chromatography-tandem mass spectrometry.An ACQUITY UPLC BEH C18 column(100 mm×2.1 mm, 1.7μm) was used, with 10 mmol/L ammonium acetate(0.1% formic acid)-methanol as mobile phase for gradient elution. In the electrospray ionization mode, positive and negative ions were used for scan at the same time. External standard method was adopted for quantitative analysis. Results The determination of 4 mycotoxins was completed within 8.0 min. In the linear ranges, the correlation coefficients of regression equations were all over 0.999. The recoveries were 82.0%-103.0% at 3 levels, and the relative standard deviations were 5.2%-9.7%. Conclusion This method is rapid, accurate and efficient, and is suitable for the simultaneous determination of 4 limited mycotoxins in wheat and its products.