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Simultaneous determination of spirodiclofen, spiromesifen, and spirotetramat and their relevant metabolites in edible fungi using ultra-performance liquid chromatography/tandem mass spectrometry
Scientific Reports ( IF 3.8 ) Pub Date : 2021-01-15 , DOI: 10.1038/s41598-021-81013-0
Fajun Tian 1 , Chengkui Qiao 1 , Caixia Wang 1 , Jing Luo 1 , Linlin Guo 1 , Tao Pang 1 , Jun Li 1 , Ruiping Wang 1 , Rongli Pang 1 , Hanzhong Xie 1
Affiliation  

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 MgSO4: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 (R2 ≥ 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−1. 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.



中文翻译:

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

开发并验证了一种快速、灵敏且可靠的分析方法,可通过超高效液相色谱/串联质谱 (UHPLC-MS/MS) 同时鉴定和定量食用真菌中的螺菌酯、螺螨酯和螺虫乙酯及其相关代谢物。首先,使用含有 1% 甲酸的乙腈进行样品萃取,然后加入 MgSO 4 :NaOAc进行相分离。然后,上清液通过伯仲胺 (PSA)、十八烷基硅烷 (C18) 和石墨化炭黑 (GCB) 纯化。所有分析物的校准线性都非常好 (R 2 ≥ 0.9953)。所有分析物均获得了可接受的回收率 (74.5–106.4%),且良好的内部和相互间标准偏差小于 14.5%。所有分析物的定量限 (LOQ) 为 10 μg kg -1。为了准确定量,应用基质匹配校准曲线来标准化基质效应。结果表明该方法适用于食用菌中3种杀螨剂及其相关代谢物的检测。

更新日期:2021-01-16
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