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采用液相色谱-串联质谱法(LC-MS/MS)测定蜂蜜和蜂产品中新型烟碱类农药及其代谢物的改良方法。

Refined methodology for the determination of neonicotinoid pesticides and their metabolites in honey bees and bee products by liquid chromatography-tandem mass spectrometry (LC-MS/MS).

机构信息

Analytical Chemistry Laboratory, Biological and Economic Analysis Division, Office of Pesticide Programs, Environmental Protection Agency 701 Mapes Road, Fort George G Meade, Maryland 20755, USA.

出版信息

J Agric Food Chem. 2010 May 26;58(10):5926-31. doi: 10.1021/jf904120n.

DOI:10.1021/jf904120n
PMID:20163114
Abstract

An analytical method was refined for the extraction and determination of neonicotinoid pesticide residues and their metabolites in honey bees and bee products. Samples were extracted with 2% triethylamine (TEA) in acetonitrile (ACN) followed by salting out, solid phase extraction (SPE) cleanup, and detection using liquid chromatography-tandem mass spectrometry (LC-MS/MS). The method was validated in triplicate at three fortification concentrations in each matrix. Good recoveries were observed for most analytes and ranged between 70 and 120% with relative standard deviations between replicates of <20% in most cases. The method limits of detection were 0.2 ng/g for the parent neonicotinoid pesticides and ranged between 0.2 and 15 ng/g for the neonicotinoid metabolites. This refined method provides lower detection limits and improved recovery of neonicotinoids and their metabolites, which will help researchers evaluate subchronic effects of these pesticides, address data gaps related to colony collapse disorder (CCD), and determine the role of pesticides in pollinator decline.

摘要

一种分析方法被改进用于提取和测定蜂蜜和蜂产品中的新烟碱类农药残留及其代谢物。样品用 2%三乙胺(TEA)在乙腈(ACN)中提取,然后进行盐析、固相萃取(SPE)净化,并用液相色谱-串联质谱(LC-MS/MS)检测。该方法在每种基质的三个加标浓度下进行了重复验证。大多数分析物的回收率良好,在大多数情况下,介于 70%至 120%之间,重复间相对标准偏差小于 20%。该方法的检出限为 0.2ng/g 的母体新烟碱类农药,0.2 至 15ng/g 的新烟碱类代谢物。这种改进的方法提供了更低的检测限和更好的新烟碱类及其代谢物的回收率,这将有助于研究人员评估这些农药的亚慢性影响,解决与蜂群崩溃失调(CCD)相关的数据空白,并确定农药在传粉媒介下降中的作用。

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