共价有机聚合物固相微萃取结合高效液相色谱-串联质谱法检测牛奶中黄曲霉毒素

Determination of aflatoxins in milk by covalent organic polymer solid phase microextraction combined with high performance liquid chromatography-tandem mass spectrometry

中文关键词:  黄曲霉毒素  牛奶  共价有机聚合物  高效液相色谱- 串联质谱

英文关键词:aflatoxin  milk  covalent organic polymer  high performance liquid chromatography-tandem mass spectrometry

中文摘要:

      目的 建立基于共价有机聚合物固相微萃取前处理结合高效液相色谱-串联质谱法(high performance liquid chromatography-tandem mass spectrometry, HPLC-MS/MS)快速、高灵敏检测牛奶中6种黄曲霉毒素残留的分析方法。方法 以1,3,5-三(4-氨苯基)苯[1,3,5-tri (4-aminophenyl) benzene, TAPB]和1,3,5-三甲酰基间苯三酚(1,3,5-triformyl-phloroglucinol, Tp)为单体制备了共价有机聚合物材料并固定在木签表面, 用于黄曲霉毒素的固相微萃取前处理。在萃取时间为20 min、洗脱溶剂为乙腈、洗脱时间为6 min条件下, 对黄曲霉毒素进行萃取和洗脱。结果 6种黄曲霉毒素在一定质量浓度范围内线性关系良好, 相关系数均大于0.9995。日内和日间精密度的相对标准偏差(relative standard deviations, RSDs)分别为4.39%~8.21%和4.97%~9.12%。将开发的方法用于实际牛奶样品中黄曲霉毒素残留检测, 加标回收率为80.01%~92.71%, RSDs为3.12%~9.54%。结论 制备的共价有机聚合物固相微萃取材料对6种黄曲霉毒素吸附性能强, 开发的固相微萃取-HPLC-MS/MS适用于牛奶中黄曲霉毒素的快速、高灵敏定量检测。

英文摘要:

      Objective To establish a rapid and highly sensitive method for the determination of 6 kinds of aflatoxins in milk by covalent organic polymer solid phase microextraction combined with high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS). Methods The 1,3,5-tri (4-aminophenyl) benzene (TAPB) and 1,3,5-triformyl-phloroglucinol (Tp) were used as monomers to prepare covalent organic polymers and fixed on the wooden tip surface, then used for solid phase microextraction pretreatment of aflatoxin. Under the conditions of extraction time of 20 minutes, elution solvent of acetonitrile, and elution time of 6 minutes, aflatoxin was extracted and eluted. Results The linear relationship of 6 kinds of aflatoxins was good in a certain mass concentration range, and the correlation coefficients were all greater than 0.9995. The relative standard deviations (RSDs) of intra-day and inter-day precision were 4.39%?8.21% and 4.97%?9.12%, respectively. The developed method was used to detect the aflatoxins residue in real milk samples. The recoveries of aflatoxins in spiked milk samples were 80.01%?92.71%, and RSDs were 3.12%?9.54%. Conclusion The prepared covalent organic polymer solid phase microextraction material has strong adsorption performance for 6 kinds of aflatoxins. The proposed solid phase microextraction-HPLC-MS/MS method is suitable for rapid and highly sensitive quantitative detection of aflatoxins in milk.