QuEChERS-液相色谱-串联质谱法测定水产品中双甲脒及其代谢物残留量

Determination of amitraz and its metabolite residues in aquatic products by QuEChERS-liquid chromatography-tandem mass spectrometry

中文关键词:  双甲脒  液相色谱-串联质谱法  水产品  QuEChERS

英文关键词:amitraz  2,4-dimethylaniline  liquid chromatography-tandem mass spectrometry  aquatic product  QuEChERS

中文摘要:

      目的 建立QuEChERS-液相色谱-串联质谱法测定水产品中双甲脒及其代谢物2,4-二甲基苯胺残留量的分析方法。方法 样品经磷酸氢二钠缓冲液调节pH后, 经乙腈提取, 盐析分层, 再通过QuEChERS方法净化, 供液相色谱-串联质谱仪测定, 内标法定量。结果 双甲脒及其代谢物的分离和洗脱在8 min内完成。在1、2、10 μg/kg 3个水平的加标浓度下, 双甲脒的平均加标回收率为108.9%~111.1%, 2,4-二甲基苯胺为100.6%~105.9%; 批内RSDs为1.4%~4.5%, 批间RSDs为8.0%~9.9%, 4种基质的批间相对标准偏差在3.1%~11.3%之间, 基质效应为–17.9%~+14.0%。方法检出限为0.5 μg/kg, 定量限为1.0 μg/kg。结论 该方法高效、准确, 适用于水产品中双甲脒及其代谢物残留量的测定, 并为相关标准制修订提供参考。

英文摘要:

      Objective To develop an analytical method for the quantification of amitraz and its metabolite 2,4-dimethylaniline residues in aquatic products using the QuEChERS coupled with liquid chromatography-tandem mass spectrometry. Methods The samples were extracted using acetonitrile after pH adjustment with a disodium hydrogen phosphate buffer, separated by salting out, and subsequently subjected to cleanup using the QuEChERS method for determination via liquid chromatography-tandem mass spectrometry. The quantification was performed using the internal standard method. Results The separation and elution of amitraz and its metabolites were successfully accomplished within a time frame of 8 minutes. The average recoveries of dimethylamidine and 2, 4-dimethylaniline were 108.9%–111.1% and 100.6%–105.9% respectively at 3 levels of 1, 2, 10 μg/kg. Between batch RSDs of 1.4%–4.5%, within the RSDs of 8.0%-9.9%. The relative standard deviations of the four substrates ranged from 3.1% to 11.3%, and the matrix effect ranged from –17.9%-+14.0%. The limits of detection and quantitation were 0.5 μg/kg and 1.0 μg/kg respectively. Conclusion The proposed method demonstrates high efficiency and accuracy in the determination of amitraz and its metabolites in aquatic products, thereby offering valuable insights for the revision of relevant standards.