同位素稀释-超高效液相色谱-串联质谱法测定谷物中隐蔽型伏马菌素  

Determination of the masked fumonisins in cereals by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry

作　　者：张烁 周爽 赵云峰 吴永宁 ZHANG Shuo;ZHOU Shuang;ZHAO Yunfeng;WU Yongning(China National Center for Food Safety Risk Assessment,Beijing 100021,China)

机构地区：[1]国家食品安全风险评估中心,北京100021

出　　处：《中国食品卫生杂志》2021年第6期680-685,共6页Chinese Journal of Food Hygiene

基　　金：国家重点研发计划(2017YFC1600304);国家自然科学基金(31801456)。

摘　　要：目的建立谷物中隐蔽型伏马菌素的同位素稀释-超高效液相色谱-串联质谱测定方法。方法谷物样品溶剂提取后,一部分稀释后用于原型伏马菌素(FBs)检测,另一部分经碱水解后经强阴离子交换(MAX)柱净化用于水解型伏马菌素(HFBs)检测。0.2%甲酸甲醇-0.2%甲酸水作为流动相梯度洗脱,CORTECS C18色谱柱(2.1 mm×100 mm, 1.6μm)分离,四极杆串联质谱仪,在电喷雾正离子化模式(ESI+)和多反应监测模式(MRM)下,同位素稀释法定量。水解型伏马菌素与游离原型伏马菌素之差即为隐蔽型伏马菌素含量。结果 FB1、FB2、FB3、HFB1、HFB2和HFB3在线性范围内相关系数(r)> 0.99;方法定量限为5.0~10μg/kg。3种谷物基质在低、中、高各水平的回收率在88.01%~114.2%之间,相对标准偏差为0.72%~11.5%。结论该方法准确、灵敏、重现性好,适用于谷物中隐蔽伏马菌素的常规检测。Objective To develop an analytical method for determination of masked fumonisins in cereals by isotope dilution-ultra high performance liquid chromatography-tandem mass spectrometry. Methods The samples were extracted and diluted for determination of parental fumonisins. Another portion of extracted samples were alkaline hydrolyzed and cleaned up using strong anionic exchange adsorbent(MAX) for determination of hydrolyzed fumonisins. The chromatographic separation was performed on a CORTECS C18 column(2.1 mm×100 mm, 1.6 μm) using 0.2% formic acid aqueous solution and methanol with 0.2% formic acid as the mobile phase under gradient elution. The six fumonisins of FB1, FB2, FB3, HFB1, HFB2 and HFB3 were analyzed by tandem mass spectrometry using multiple reactions monitoring(MRM) mode. The isotope dilution method was applied for quantitative analysis. Results The six fumonisins showed good linearity with relative coefficients above 0.99. Limits of quantitation(LOQs) were in the range of 5.0-10 μg/kg. At the low, medium and high-spiked levels, the recoveries of fumonisins in three types of cereals were from 88.01% to 114.21%, with precision(RSD) of 0.72%-11.5%. Conclusion This method is accurate, sensitive and reproducible for the determination of masked fumonisins in cereals. It is suitable for the routine test in analytical chemistry laboratories for monitoring masked fumonisins levels in cereals.

关 键 词：谷物 高效液相色谱-串联质谱法 隐蔽型伏马毒素 同位素稀释 碱水解 

分 类 号：R155[医药卫生—营养与食品卫生学]