超高效液相色谱-四极杆串联离子阱复合质谱法筛查和定量玉米中5种链格孢菌毒素

Screening and quantitation of 5 kinds of Alternaria toxins in maize by ultra performance liquid chromatography-Q-trap-tandem mass spectrometry

中文关键词:  超高效液相色谱-四极杆串联离子阱复合质谱法  链格孢菌毒素  玉米  筛查  定量

英文关键词:ultra performance liquid chromatography-Q-trap-tandem mass spectrometry  Alternaria toxins  maize  screening  quantitation

中文摘要:

      目的 建立超高效液相色谱-四极杆串联离子阱复合质谱法(ultra performance liquid chromatography-Q-trap-tandem mass spectrometry, UPLC-Q-Trap-MS)对玉米中的5种链格孢菌毒素同时进行筛查和定量的分析方法。方法 使用改进型QuEChERS法对玉米样品进行提取和净化, 以多反应监测(multiple reaction monitoring, MRM)作为探针检测, 并通过信息依赖性采集(information dependent acquisition, IDA)触发增强型子离子扫描(enhanced product ion scan, EPI)模式, 采用外标法定量。结果 玉米中5种链格孢菌毒素的检出限为0.017~0.720 μg/kg, 定量限为0.057~2.400 μg/kg, 并且在1.0~200.0 ng/mL的线性范围内良好, 相关系数r≥0.9929。在样品基质中分别添加20、40和200 μg/kg 3个水平的标准品进行加标回收试验, 5种链格孢菌毒素的平均回收率为80.6%~104.7%, 相对标准偏差(relative standard deviations, RSDs)为1.57%~8.27% (n=6)。结论 该方法具有操作简单、灵敏度高、准确度高的特点, 适合于玉米中5种链格孢菌毒素的同时快速筛查与准确定量。

英文摘要:

      Objective To establish a method for the simultaneous screening and quantitation of 5 kinds of Alternaria toxins in maize by ultra performance liquid chromatography-Q-trap-tandem mass spectrometry (UPLC-Q-Trap-MS). Methods Maize samples were extracted and purified using the modified QuEChERS method, multiple reaction monitoring (MRM) was used as the probe detection, and enhanced product ion scan (EPI) mode was triggered by information dependent acquisition (IDA) and quantified by the external standard method. Results The limits of detection the 5 kinds of Alternaria toxins in maize were 0.017?0.720 μg/kg, and the limits of quantitation were 0.057?2.400 μg/kg, the linearities were good in the range of 1.0?200.0 ng/mL, with the correlation coefficients r≥0.9929. The standard samples at levels of 20, 40 and 200 μg/kg were added into the sample matrix for the spiked recovery experiments, the average recoveries of the 5 kinds of Alternaria toxins were 80.6%?104.7%, and the relative standard deviations (RSDs) were 1.57%?8.27% (n=6). Conclusion The method has the characteristics of simple operation, high sensitivity and high accuracy, which is suitable for rapid screening and accurate quantification of 5 kinds of Alternaria toxins in maize.