Determination of spinetoram and its metabolites in amaranth and parsley using QuEChERS-based extraction and liquid chromatography-tandem mass spectrometry

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• 作者：Ki Hun Park^a ; ¹ ; Jeong-Heui Choi^a ; ¹ ; A.M. Abd El-Aty^b ; ^{abdelaty44@hotmail.com} ; Soon-Kil Cho^c ; Jong-Hyouk Park^a ; Bo Mi Kim^a ; Angel Yang^a ; Tae Woong Na^a ; Md. Musfiqur Rahman^a ; Geon-Jae Im^d ; Jae-Han Shim^a ; ^{jhshim@chonnam.ac.kr}
• 关键词：Simultaneous determination ; Spinetoram ; Metabolites ; Minor crops ; LC&ndash ; ESI&ndash ; MS/MS
• 刊名：Food Chemistry
• 出版年：2012
• 期刊代码：48_03088146
• 类别：abs
• 出版时间：15 October, 2012
• 卷：134
• 期：4
• 页码：2552-2559
• 文件大小：1101 K

摘要

In this study, a simultaneous method was developed for the determination of spinetoram (XDE-175-J and XDE-175-L) and its demethyl metabolites (N-demethyl-175-J and N-demethyl-175-L) and formyl metabolites (N-formyl-175-J and N-formyl-175-L) in the minor crops; amaranth and parsley. The method uses quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based extraction. Afterwards, the analytes were quantified and confirmed via liquid chromatography-electrospray ionisation tandem mass spectrometry (LC-ESI-MS/MS) in the positive ion mode using multiple reaction monitoring (MRM). Calibration curves were linear over the calibration ranges for all the analytes tested with r² > 0.993. Limits of detection and quantitation were 0.01 and 0.03 mg/kg for all the tested analytes in amaranth and parsley, respectively. Recovery values, at spiking levels 0.05 and 0.25 mg/kg, ranged from 71.0%to 115.2%with relative standard deviations <15%, except for N-formyl-175-J in both amaranth and parsley. This method was applied to field-incurred samples and was shown to provide an adequate sensitivity and performance for the simultaneous determination of spinetoram and metabolites. To the best of our knowledge, this is the first time spinetoram and its metabolites were quantified using LC-MS/MS in minor crops.