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

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C_(18)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0.005~0.500mg/L范围内线性关系好(r^(2)>0.99),检出限为0.005mg/kg,定量限为0.01mg/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。

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 C_(18) 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(r^(2)>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.