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超高效液相色谱/串联质谱法同时测定食用菌中螺虫乙酯、螺甲螨酯和螺螨酯及其相关代谢物

Simultaneous determination of spirodiclofen, spiromesifen, and spirotetramat and their relevant metabolites in edible fungi using ultra-performance liquid chromatography/tandem mass spectrometry.

机构信息

Zhengzhou Fruit Research Institute, Chinese Academy of Agricultural Sciences, Zhengzhou, 450009, China.

出版信息

Sci Rep. 2021 Jan 15;11(1):1547. doi: 10.1038/s41598-021-81013-0.

Abstract

A fast, sensitive, and reliable analytical method was developed and validated for simultaneous identification and quantification of spirodiclofen, spiromesifen, and spirotetramat and their relevant metabolites in edible fungi by ultra-performance liquid chromatography/tandem mass spectrometry (UHPLC-MS/MS). First, sample extraction was done with acetonitrile containing 1% formic acid followed by phase separation with the addition of MgSO:NaOAc. Then, the supernatant was purified by primary secondary amine (PSA), octadecylsilane (C18), and graphitized carbon black (GCB). The linearities of the calibrations for all analytes were excellent (R ≥ 0.9953). Acceptable recoveries (74.5-106.4%) for all analytes were obtained with good intra- and inter- relative standard deviations of less than 14.5%. The limit of quantification (LOQs) for all analytes was 10 μg kg. For accurate quantification, matrix-matched calibration curve was applied to normalize the matrix effect. The results indicated that the method was suitable for detecting the three acaricides and their relevant metabolites in edible fungi.

摘要

建立并验证了一种超高效液相色谱-串联质谱法(UHPLC-MS/MS),用于同时鉴定和定量食用菌中螺虫乙酯、螺甲螨酯和螺螨酯及其相关代谢物。首先,用含 1%甲酸的乙腈提取样品,然后加入 MgSO₄-NaOAc 进行液-液萃取分离。然后,用初级二级胺(PSA)、十八烷基硅烷(C18)和石墨化炭黑(GCB)对上清液进行净化。所有分析物的校准曲线线性良好(R ≥ 0.9953)。所有分析物的回收率均在 74.5-106.4%之间,日内和日间相对标准偏差均小于 14.5%。所有分析物的定量限(LOQs)均为 10 μg kg。为了进行准确的定量分析,采用基质匹配校准曲线来归一化基质效应。结果表明,该方法适用于检测食用菌中的三种杀螨剂及其相关代谢物。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/b215/7810688/f842a05831a6/41598_2021_81013_Fig1_HTML.jpg

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