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采用加压溶剂萃取和液相色谱-串联质谱法测定牛组织中的新烟碱类杀虫剂残留。

Determination of neonicotinoid insecticides residues in bovine tissues by pressurized solvent extraction and liquid chromatography-tandem mass spectrometry.

机构信息

Department of Pharmacology and Toxicology, College of Veterinary Medicine, China Agricultural University, Beijing 100193, China.

出版信息

J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jan 1;879(1):117-22. doi: 10.1016/j.jchromb.2010.11.008. Epub 2010 Nov 19.

Abstract

A rapid, sensitive, and environmental-friendly method has been developed for the simultaneous determination of seven neonicotinoid insecticides residues in bovine muscle and liver. The sample preparation procedure was based on a high automated pressurized solvent extraction (PSE) combined with solid-phase extraction (SPE) clean-up. The target compounds were identified and quantitatively determined by liquid chromatography coupled with electrospray ionization tandem mass spectrometry (LC-ESI-MS/MS) operated in multiple reaction monitoring mode. Average recoveries of the seven analytes from fortified samples ranged between 83.2% and 101.9%, with relative standard deviations (RSDs) lower than 10.8%. The limits of detection (LODs) and quantification (LOQs) for neonicotinoids were in the ranges of 0.8-1.5 μgkg⁻¹ and 2.5-5.0 μgkg⁻¹, respectively. This validated method was successively applied to the determination of neonicotinoid insecticides in real samples from markets.

摘要

已开发出一种快速、灵敏且环境友好的方法,用于同时测定牛肌肉和肝脏中七种新烟碱类杀虫剂残留。样品制备程序基于自动化加压溶剂萃取(PSE)与固相萃取(SPE)净化相结合。通过液相色谱-电喷雾串联质谱(LC-ESI-MS/MS)在多反应监测模式下对目标化合物进行鉴定和定量测定。七种分析物从加标样品中的平均回收率在 83.2%至 101.9%之间,相对标准偏差(RSD)低于 10.8%。新烟碱类杀虫剂的检出限(LOD)和定量限(LOQ)分别在 0.8-1.5 μgkg⁻¹和 2.5-5.0 μgkg⁻¹范围内。该经验证的方法成功应用于市场中实际样品中新型烟碱类杀虫剂的测定。

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