超高效液相色谱-串联质谱法同时检测饲料原料、饲料成品中18种真菌毒素含量

Simultaneous determination of 18 kinds of mycotoxins in feed ingredients and feed products by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱法  饲料  真菌毒素

英文关键词:ultra performance liquid chromatography-tandem mass spectrometry  feed  mycotoxin

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定饲料原料和饲料成品中18种真菌毒素的方法。方法 样品经50%乙腈水溶液提取后, 经MycoSpin TM 400净化柱净化, 同位素内标稀释后, 上机测定。结果 在低、中、高3个添加水平下, 18种毒素的空白样品平均加标回收率为62.6%~112.53%(预混料除外), 相对标准偏差(relative standard deviation, RSD)为1.82%~13.83%。18种真菌毒素在各自的线性范围内线性关系良好, 线性系数均大于0.995, 检出限(limit of detection, LOD, S/N=3)和定量限(limit of quantity, LOQ, S/N=10)分别为0.15~10 μg/L和0.5~30 μg/L。对2018年初的饲料原料以及饲料成品近900个样品进行了18种真菌毒素的普查工作, 结果显示呕吐毒素和伏马菌素的阳性检出率最高, 分别为93%和91%。结论 此方法操作简单、灵敏度高且应用范围广, 可以用于饲料中真菌毒素的大规模普查。

英文摘要:

      Objective To establish a method for simultaneous determination of 18 kinds of mycotoxins in feed raw materials and feed products by ultra performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted with 50% acetonitrile aqueous solution, purified by MycoSpinTM 400 purification column, diluted by the isotope internal standard, and determined by UPLC-MS/MS. Results The recoveries at low, medium and high levels were 62.6%-112.53% (except premix), and the relative standard deviations (RSDs) were 1.82%-13.83%. The 18 kinds of mycotoxins had good linear relationships in their linear ranges, the linear coefficients were all greater than 0.995, the limits of detection (LODs, S/N=3) and the limits of quantity (LOQs, S/N=10) were 0.1510 μg/L and 0.5-30 μg/L, respectively. A total of 18 mycotoxin surveys were conducted in nearly 900 samples of feed raw materials and feed products in early 2018, and the results showed that the positive detection rates of vomiting toxin and fumonisin were the highest of 93% and 91%, respectively. Conclusion This method is simple in operation, high in sensitivity and wide in application, which can be used for large-scale screening of mycotoxins in feed.