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土壤中聚乙醛定量分析方法的开发与验证

Analytical method development and validation for the quantification of metaldehyde in soil.

作者信息

Keighley Nathan, Ramwell Carmel, Werner David, Sinclair Chris

机构信息

Fera Science Ltd. York Biotech Campus, Sand Hutton, York YO41 1LZ, UK.

School of Engineering, Newcastle University, Newcastle upon Tyne NE1 7RU, UK.

出版信息

MethodsX. 2021 Aug 8;8:101482. doi: 10.1016/j.mex.2021.101482. eCollection 2021.

Abstract

Previously published methods for the analysis of metaldehyde were adapted for its reliable quantification in soil extracts. Varied methanol-water extraction solvents were trialed, but the use of pure methanol proved to be the most reliable approach for the scaled down methodology. Analysis of metaldehyde was done using LC-MS. Initially the method had problems with matrix suppression of the signal. The method was therefore further developed to overcome this challenge to avoid the costs and time demands of laborious clean-up protocols. This modification to the method involved use of the BEH Phenyl column instead of the C column initially used, and optimization of the gradient flow of the mobile phase. The optimized LC-MS method was validated and used for further research applications. In brief,•We investigated the recovery of metaldehyde from spiked soil samples.•The optimized LC-MS method achieved acceptable metaldehyde recoveries (100-132%, 109% on average) for a range of soil types.•The optimized method was suitable for high through-put analyzes.

摘要

先前发表的分析聚乙醛的方法被调整用于在土壤提取物中对其进行可靠定量。试验了多种甲醇 - 水萃取溶剂,但事实证明,对于按比例缩小的方法,使用纯甲醇是最可靠的方法。使用液相色谱 - 质谱联用仪(LC-MS)对聚乙醛进行分析。最初,该方法存在信号基质抑制问题。因此,对该方法进行了进一步改进,以克服这一挑战,避免繁琐净化方案所需的成本和时间。对该方法的改进包括使用BEH苯基柱代替最初使用的C柱,并优化流动相的梯度流速。经过验证的优化LC-MS方法被用于进一步的研究应用。简而言之,•我们研究了加标土壤样品中聚乙醛的回收率。•优化后的LC-MS方法在一系列土壤类型中实现了可接受的聚乙醛回收率(100 - 132%,平均109%)。•优化后的方法适用于高通量分析。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/6a9f/8374715/5d3da75c04ad/ga1.jpg

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