超高效液相色谱-串联质谱法快速检测动物饲料中5种霉菌毒素

Rapid simultaneous determination of 5 mycotoxins in animal feed by ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  霉菌毒素  固相萃取  超高效液相色谱-串联质谱法  饲料

英文关键词:mycotoxins  solid phase extraction  ultra performance liquid chromatography-tandem mass spectrometry  feed

中文摘要:

      目的 建立一种同步、快速的测定饲料中5种主要霉菌毒素的超高效液相色谱-串联质谱(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)检测方法。方法 样品经84%乙腈水(含0.1%甲酸)提取液提取, MLJ-1杂质吸附型固相萃取柱净化。采用0.1 mmol/L乙酸铵/0.1%甲酸-水(A)和0.1%甲酸-甲醇(B)作为流动相进行梯度洗脱, 质谱采用多反应监测模式(multiple reaction monitoring, MRM)对霉菌毒素及其同位素内标的定量离子和定性离子进行监测。结果 本方法在1 min内完成样品净化处理, 15 min内完成5种目标化合物的分离分析。5种霉菌毒素在高、中和低浓度添加水平的回收率为83.9%~113.8%, 相对标准偏差为0.6%~15.0%(n=6), 方法定量限为0.3~4.0 μg/kg。结论 该方法操作简单、快速, 适合饲料中5种主要霉菌毒素同步确证检测。

英文摘要:

      Objective To establish a rapid method for simultaneous determination of 5 major mycotoxins in animal feed samples by ultra performance liquid chromatography-tandem mass spectrometry (UPLC–MS/MS). Methods The 5 analytes were extracted from the feed samples by acetonitrile-water-formic acid, and purified by a commercial MLJ-1 pass-through solid-phase extraction (SPE) clean-up cartridge, and then analyzed by UPLC-MS/MS. The 5 analytes were then separated on a reversed phase column using a gradient elution program of 0.1 mmol/L ammonium acetate/0.1% formic acid aqueous solution and 0.1% formic acid methanol solution. The quantitative and qualitative ions of mycotoxin and their internal isotopes were detected with multiple reaction monitoring (MRM) mode. Results This method could purify the samples within 1 min and separate and analyze 5 target compounds within 15 min. The recoveries of 3 spiked levels were in range of 83.9%-113.8%, with the relative standard deviations (RSDs) of 0.6%-15.0% (n=6). The limits of quantification (LOQ) for all analytes were between 0.3 and 4.0 μg/kg. Conclusion The proposed method is simple, rapid and accurate, which is suitable for detecting 5 major mycotoxins in animal feed samples.