分散固相萃取净化-超高效液相色谱-串联质谱法同时测定水果中7种链格孢霉毒素的含量

Simultaneous determination of 7 kinds of Alternaria mycotoxins in fruits by dispersive solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  链格孢霉毒素  分散固相萃取  超高效液相色谱-串联质谱

英文关键词:Alternaria mytoxins  dispersive solid-phase extraction  ultra performance liquid chromatography- tandem mass spectrometry

中文摘要:

      目的 建立分散固相萃取净化-超高效液相色谱-串联质谱法快速、准确地同时检测水果中7种链格孢霉毒素的方法。方法 试样用酸化乙腈提取, 无水硫酸镁除水, 氯化钠盐析, 上层清液经C18与石墨化碳黑分散固相萃取净化后, 采用超高效液相色谱-串联质谱法测定, 基质匹配标准溶液外标法定量。结果 7种链格孢霉毒素在0.005~0.500 mg/L范围内线性关系好(r2>0.99), 检出限为0.005 mg/kg, 定量限为0.01 mg/kg, 回收率在77.30%~114.34%之间, 批内相对标准偏差为0.65%~14.81%, 批间相对标准偏差为0.03%~18.59%。结论 该方法简单、高效, 精密度及准确度高, 适用于水果中7种链格孢霉毒素的测定。

英文摘要:

      Objective To develop a rapid and accurate method for the simultaneous determination of 7 kinds of Alternaria mycotoxins by dispersive solid phase extraction combined with ultra performance liquid chromatography-tandem mass spectrometry in fruits. Methods Samples were extracted with acidified acetonitrile, dehydrated by anhydrous magnesium sulfate and salted out with sodium chloride, and the supernatant was cleaned up by dispersive solid-phase extraction with C18 and graphitized carbon black. Then determined by ultra performance liquid chromatography-tandem mass spectrometry, quantitatived by substrate matching and external standard calibration method. Results The linearity of the method was good in the range of 0.005~0.500 mg/L (r2＞0.99) and the limits of detection were 0.005 mg/kg, the limits of quantification were 0.01 mg/kg. The recoveries ranged from 77.30% to 114.34% with the relative standard deviation within batches from 0.65% to 14.81% and the relative standard deviation between batches from 0.03% to 18.59%. Conclusion The method is simple, efficient, precise and accurate and can be used for the determination of the 7 kinds of Alternaria mycotoxins in fruits.