盐酸吗啉胍在7种植物源基质中残留分析方法的建立及其在烟草中残留特征解析

Development of an Analytical Method for the Residue of Moroxydine in Plant-Derived Matrix and the Dissipation in Tobacco

摘要: 目的：建立SPE-超高效液相色谱–串联质谱法检测植物源性食品中盐酸吗啉胍残留的分析方法。方法：样品经三氯乙酸提取，PEP固相萃取柱净化后，以超高效液相色谱–串联质谱检测，外标法定量。对提取溶剂、净化条件进行了优化。结果：在0.01、0.5和5 mg/kg添加水平下，以最低添加水平0.01 mg/kg作为定量限(LOQ)，各基质的平均回收率为75.1%~95.4%，相对标准偏差为1.0%~12.0%，重现性范围为5.1%~9.8%。该方法应用于烟草田间盐酸吗啉胍的残留特性研究，结果显示，盐酸吗啉胍在广西、贵州、湖南和云南四省鲜烟叶中的半衰期分别为21.0、15.8、9.8和7.7天，干烟叶的半衰期为19.3、12.8、8.3、7.7天。结论：该方法准确度和灵敏度高、重现性好，适用于烟草、番茄、辣椒等植物源基质中盐酸吗啉胍的残留检测，其消解动态数据为盐酸吗啉胍的在烟草上的合理使用提供了参考依据，也为我国制定其在烟草上的最大残留限量提供了重要数据参考。

Abstract: Aims: To establish a SPE-ultra-high performance liquid chromatography-tandem mass spectrometry method for detecting moroxydine residues in plant-derived foods. [Methods Samples were extracted with trichloroacetic acid, purified using PEP solid-phase extraction columns, and analysed by ultra-high performance liquid chromatography-tandem mass spectrometry with external standard quantification. Extraction solvents and purification were optimised. Results: At spiked levels of 0.01, 0.5, and 5 mg/kg, the limit of quantification (LOQ) was set at the lowest spiked level of 0.01 mg/kg. Average recovery rates ranged from 75.1% to 95.4% across matrices, with relative standard deviations (RSD) between 1.0% and 12.0% and reproducibility ranges from 5.1% to 9.8%. This method was applied to investigate the residue characteristics of moroxydine in tobacco fields. Results indicated half-lives of 21.0, 15.8, 9.8, and 7.7 days for fresh tobacco leaves in Guangxi, Guizhou, Hunan, and Yunnan provinces respectively, with half-lives of 19.3, 12.8, 8.3, and 7.7 days for dried tobacco leaves. Conclusion: The method has high accuracy, high sensitivity and good reproducibility, and is suitable for the detection of moroxydine residues in plant-derived matrices such as tobacco, tomatoes, and peppers. Its digestion kinetic data provide a reference basis for the rational application of moroxydine in tobacco cultivation and provides reference data for the rational use and registration of moroxydine.