超高效液相色谱-串联质谱法测定婴幼儿谷物辅食中的T-2和HT-2真菌毒素

Determination of T-2 and HT-2 mycotoxins in infant cereal food by ultra-high performance liquid chromatography-tandem mass spectrometry

中文关键词:  超高效液相色谱-串联质谱  谷物  真菌毒素

英文关键词:ultra-high performance liquid chromatography-tandem mass spectrometry  cereal  mycotoxin

中文摘要:

      目的 建立检测婴幼儿谷物辅食中T-2和HT-2真菌毒素的超高效液相色谱—串联质谱分析方法。 方法 婴幼儿营养面条等谷物样品用84%乙腈水溶液涡旋振荡提取, 经多功能净化柱净化后氮吹浓缩, 以甲醇和超纯水为流动相, 经Waters ACQUITY BEH C18色谱柱梯度洗脱分离, 采用电喷雾离子源, 多反应监测(multiple reaction monitoring, MRM)正离子模式进行检测, 内标法定量。结果 T-2和HT-2真菌毒素在0.500 ~200 ng/mL范围内线性关系良好, 相关系数(r)>0.999, 方法检出限分别为0.03 μg/kg和0.05 μg/kg, 方法定量限分别为0.10 μg/kg和0.15 μg/kg, 不同浓度水平的加标平均回收率(n=6)为92.3%~99.4%和90.2%~96.2%, 相对标准偏差为3.0%~4.2%和2.8%~4.7%。结论 本方法前处理方法简单, 灵敏度高、重现性好, 可应用于婴幼儿谷物辅食中T-2和HT-2真菌毒素残留的确证和定量分析。

英文摘要:

      Objective To establish a method for determination of T-2 and HT-2 mycotoxins in infant cereal food by ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods Samples were sequentially extracted with 84% acetonitrile, concentrated with nitrogen and purified by multifunction cleaning column. T-2 and HT-2 were separated by Waters ACQUITY BEH C18 chromatographic column with mobile phase of methanol and ultrapure water. Analytes were performed by electrospray ionization (ESI) in positive mode of multiple reaction monitoring (MRM). Quantification was performed by the internal standard method. Results T-2 and HT-2 had good linear relationships in 0.500 ~200 ng/mL, with the correlation coefficients above 0.999. The limits of detection were 0.03 μg/kg and 0.05 μg/kg, and the limits of quantitation were 0.10 μg/kg and 0.15 μg/kg, respectively. The average recoveries at different concentration levels were among 92.3%~99.4% and 90.2%~96.2% (n=6), and their relative standard deviations were 3.0%~4.2% and 2.8%~4.7%, respectively. Conclusion The method is simple, sensitive and repeatable, which is suitable for confirmation and quantitative analysis of T-2 and HT-2 mycotoxins in infant cereal food.