动物源性食品中烯草酮及代谢物烯草酮砜和烯草酮亚砜残留分析方法

    Analysis method for residues of clethodim and its metabolites clethodim sulfone and clethodim sulfoxide in animal origin foods

    • 摘要: 农药不合理使用导致的残留问题在动物源性食品中时有发生,其对人类健康的潜在风险正日益受到关注。本研究开发了一种基于超高效液相色谱-串联质谱(UPLC-MS/MS)同时检测猪肉、鸡肝和牛奶样品中烯草酮及代谢物烯草酮砜和烯草酮亚砜残留的方法。样品中烯草酮及代谢物经乙腈提取后,通过正己烷液-液分配和C18固相分散净化。结果表明,该方法中烯草酮及代谢物在猪肉、鸡肝和牛奶基质中均展现了良好的线性关系(R2 ≥ 0.9956),定量限 (LOQ) 分别为0.01、0.01和0.005 mg/L。该方法的添加回收率在84%~108%之间,相对标准偏差 (RSD) 在1%~10%之间。与其他文献报道的方法相比,该方法减少了有机溶剂的消耗,提高了灵敏度。采用所建立的方法,对从全国超市抽取的共90份猪肉、鸡肝和牛奶样本进行了检测,均未检测出烯草酮及其代谢物烯草酮砜和烯草酮亚砜残留。研究结果可为我国动物源性食品中烯草酮及代谢物标准检测方法的制定提供参考。

       

      Abstract: The residue issues resulting from improper use of pesticides occurs frequently in animal origin foods, and its potential risks to human health have drawn attention gradually. This study developed a method based on ultra-high performance liquid chromatography-tandem mass spectrometry (UPLC-MS/MS) for the simultaneous detection of clethodim and its metabolites, clethodim sulfone and clethodim sulfoxide, in pork, chicken liver, and milk samples. The samples were extracted with acetonitrile, followed by liquid-liquid partitioning with n-hexane and purification with C18 solid-phase dispersion. The results showed that clethodim and its metabolites exhibited good linearity in pork, chicken liver, and milk (R² ≥ 0.9956), with limits of quantification (LOQ) of 0.01, 0.01, and 0.005 mg/L, respectively. The recovery of the method ranged from 84% to 108%, with relative standard deviations (RSD) between 1% and 10%. Compared with other reported methods, the developed method reduced the consumption of organic solvent and achieved higher sensitivity. The established method was used to detect 90 samples of pork, chicken liver, and milk that collected from supermarkets across the country, and no residues of clethodim or its metabolites, clethodim sulfone and clethodim sulfoxide, were detected. The results provide reference for the establishment of standard detection methods for clethodim and its metabolites in animal-derived samples in China.

       

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