壳聚糖净化-超高效液相色谱-三重四极杆/复合线性离子阱质谱法测定水产品中硝基呋喃类代谢物残留研究

Determination of nitrofuran metabolites in aquatic products by chitosan purification-ultra performance liquid chromatography-quadrupole linear ion trap-mass spectrometry

中文关键词:  壳聚糖  水产品  硝基呋喃类代谢物  超高效液相色谱-串联质谱法

英文关键词:chitosan  aquatic products  nitrofuran metabolites  ultra performance liquid chromatography- quadrupole linear ion trap-mass spectrometry

中文摘要:

      目的 建立一种基于壳聚糖净化结合超高效液相色谱-三重四极杆/复合线性离子阱质谱法, 测定水产品中硝基呋喃类代谢物残留的快速检测方法。方法 样品经盐酸水解、2-硝基苯甲醛衍生、乙酸乙酯提取、壳聚糖净化、氮吹浓缩复溶后, 借助超高效液相色谱仪实现快速分离, 三重四极杆/复合线性离子阱质谱仪进行测定, 内标法定量分析, 实现快速、准确地测定水产品中硝基呋喃类代谢物残留量。结果 4种硝基呋喃类代谢物在0.5~10.0 μg/L质量浓度范围内线性关系良好, 相关系数均大于0.998, 定量限为0.5 μg/kg; 以鲤鱼、大菱鲆以及南美白对虾为样品, 在3个不同添加水平下4种硝基呋喃类代谢物的平均回收率为96.5%~116.5%, 日内相对标准偏差为2.2%~9.3%, 日间相对标准偏差为2.7%~9.7%。结论 该方法经济、简便、高效, 灵敏度高, 重复性好, 可作为水产品中4种硝基呋喃类代谢物残留的常规检测方法。

英文摘要:

      Objective To develop a rapid method for the determination of nitrofuran metabolites in aquatic products based on chitosan purification combined with ultra performance liquid chromatography and triple quadrupole/composite linear ion trap mass spectrometer. Methods The samples were hydrolyzed by hydrochloric acid, derived by 2-nitrobenzaldehyde, extracted by ethyl acetate, rapidly purified by chitosan, and then concentrated and redissolved. Rapid separation was achieved by ultra performance liquid chromatography, measured by triple quadrupole/composite linear ion trap mass spectrometer, and quantified by internal standard method to achieve the rapid and accurate determination of nitrofuran metabolites residues in aquatic products. Results The 4 kinds of nitrofuran metabolites had a good linear relationship in the concentration range of 0.5–10.0 μg/L, the correlation coefficients were all more than 0.998, and the limit of quantification was 0.5 μg/kg. Taking carp, Scophthalmus maximus and Litopenaeus vannamei as samples, the average recovery of 4 kinds of nitrofuran metabolites at 3 different addition levels was 96.5%–116.5%, the intra-day relative standard deviation was 2.2%–9.3%, and the intra-day relative standard deviation was 2.7%–9.7%. Conclusion The method is economical, simple, efficient, sensitive and reproducible, and can be used as a routine method for the determination of 4 kinds of nitrofuran metabolites in aquatic products.