同位素稀释-超高效液相色谱-串联质谱法同时测定婴幼儿谷类辅助食品中的15种真菌毒素和6种农药残留

Simultaneous determination of 15 kinds of mycotoxins and 6 kinds of pesticide residues in cereal-based complementary foods for infants and young children by isotope dilution-ultra performance liquid chromatography-tandem mass spectrometry

中文关键词:  同位素稀释  超高效液相色谱-串联质谱法  婴幼儿谷类辅助食品  真菌毒素  农药残留

英文关键词:isotope dilution  ultra performance liquid chromatography-tandem mass spectrometry  cereal-based complementary foods for infants and young children  mycotoxins  pesticide residues

中文摘要:

      目的 建立超高效液相色谱-串联质谱法(ultra performance liquid chromatography-tandem mass spectrometry, UPLC-MS/MS)同时测定婴幼儿谷类辅助食品中15种真菌毒素和6种农药残留的方法。方法 样品经乙腈-水-甲酸(84:15:1, V:V:V)提取并低温高速离心后, 直接用水稀释提取液, 以BEH C18为分离柱, 利用UPLC-MS/MS测定, 在多反应监测模式下同位素内标法定量。结果 在最佳实验条件下, 目标物在各自线性范围内线性良好, 相关系数(r)均大于0.999; 检出限为0.03~7.00 μg/kg, 定量限为0.10~23.00 μg/kg; 加标回收率在75.0%~108.0%之间, 相对标准偏差为2.8%~11.0%。结论 该方法前处理简单快速、灵敏度高, 有效解决基质效应问题, 适用于大批量婴幼儿谷类辅助食品中15种真菌毒素和6种农药残留的同时测定。

英文摘要:

      Objective To establish a method for the simultaneous determination of 15 kinds of mycotoxins and 6 kinds of pesticide residues in cereal-based complementary foods for infants and young children by ultra performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS). Methods After the sample was extracted with acetonitrile-water-formic acid (84:15:1, V:V:V) and centrifuged at low temperature and high speed, the extracted components were directly diluted with water. The extracted components were separated on a BEH C18, and detected by UPLC-MS/MS in multi-reaction monitoring mode. The isotopic internal standard method was used for quantitative analysis. Results Under the optimum operation conditions, the target compounds showed good linearity in their respective linear ranges with the correlation coefficients (r) more than 0.999. The limits of detection and limits of quantification were 0.03?7.00 μg/kg and 0.10?23.00 μg/kg, respectively. The recoveries ranged from 75.0% to 108.0% with the relative standard deviation of 2.8%?11.0%. Conclusion This method has the advantages of simple and rapid pretreatment as well as high sensitivity, and can reduce the influence of matrix effect. It is suitable for the simultaneous determination of 15 kinds of mycotoxins and 6 kinds of pesticide residues in large quantities of cereal-based complementary foods for infants and young children.