QuEChERS-超高效液相色谱-串联质谱法测定小麦粉中4种交链孢霉菌素

Determination of 4 kinds of Alternaria toxins in wheat flour by QuEChERS- ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  交链孢霉菌素  超高效液相色谱-串联质谱法  QuEChERS  小麦粉

英文关键词:Alternaria toxins  ultra performance liquid chromatography-tandem mass spectrometry  QuEChERS  wheat flour

中文摘要:

      目的 建立QuEChERS-超高效液相色谱-串联质谱法测定小麦粉中4种交链孢霉菌素含量。方法 样品以丙酮为提取剂, 经QuEChERS法前处理, 采用Endeavorsil C18色谱柱(2.1 mm×100 mm, 1.8 μm), 以甲醇-1.5 mmol/L碳酸氢铵为流动相, 梯度洗脱, 多反应监测模式检测, 细交链孢菌酮酸含量采用内标法定量, 交链孢酚、腾毒素和交链孢酚单甲醚含量采用外标法定量。结果 该方法对4种交链孢霉菌素有很好的分离效果, 检出限为0.06~0.50 μg/kg, 回收率为85.4%~104.3%, 相对标准偏差为2.3%~9.8%, 相关系数≥0.9990。 结论 本方法简便、快速, 灵敏度、精密度、回收率均满足方法学要求, 适用于小麦粉中4种交链孢霉菌素含量的同时测定。

英文摘要:

      Objective To establish a method for determination of 4 kinds of Alternaria toxins in wheat flour by QuEChERS-ultra performance liquid chromatography-tandem mass spectrometry (QuEChERS-UPLC-MS/MS). Methods The samples were extracted with acetone, pertreated by QuEChERS method. The analysis was achieved with a Endeavorsil C18 column (2.1 mm×100 mm, 1.8 μm) by gradient elution using 0.1% methanol and 1.5 mmol/L ammonium bicarbonate. The detection was carried out by multiple reactions monitoring. The tenuazonic acid content was quantitatively analyzed by internal standard method and the contents of alternariol, tentoxin and alternariol monomethyl ether were quantified by external standard method. Results This method had a good separation effect on 4 kinds of Alternaria toxins. The limit of detections were 0.06-0.50 μg/kg, and the recoveries were 85.4%-104.3%. The relative standard deviations were 2.3%-9.8% with the correlation coefficients above 0.9990. Conclusion This method is simple and rapid, and its sensitivity, precision and recovery are all satisfied with the methodological requirements, which is suitable for the simultaneous determination of 4 kinds of Alternaria toxins in wheat flour.