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

• Published in: Food chemistry 2012-10, Vol.134 (4), p.2552-2559
• Main Authors: Park, Ki Hun, Choi, Jeong-Heui, Abd El-Aty, A.M., Cho, Soon-Kil, Park, Jong-Hyouk, Kim, Bo Mi, Yang, Angel, Na, Tae Woong, Musfiqur Rahman, Md, Im, Geon-Jae, Shim, Jae-Han
• Format: Article
• Language: English
• Subjects: Amaranthus; Amaranthus - chemistry; Amaranthus - metabolism; Biological and medical sciences; Cereal and baking product industries; Chromatography, High Pressure Liquid - methods; detection limit; Food Contamination - analysis; Food engineering; Food industries; Fundamental and applied biological sciences. Psychology; General aspects; Insecticides - chemistry; Insecticides - isolation & purification; Insecticides - metabolism; ionization; LC–ESI–MS/MS; Macrolides - chemistry; Macrolides - isolation & purification; Macrolides - metabolism; mass spectrometry; Metabolites; Minor crops; monitoring; parsley; Petroselinum - chemistry; Petroselinum - metabolism; quantitative analysis; Simultaneous determination; Solid Phase Extraction - methods; specialty crops; Spinetoram; Tandem Mass Spectrometry - methods
• ISSN: 0308-8146; 1873-7072
• DOI: 10.1016/j.foodchem.2012.04.066

► A simultaneous method was developed for the determination of spinetoram and its metabolites. ► LC–ESI–MS/MS in positive ion mode using MRM was used for confirmation and quantification. ► The method provides an adequate sensitivity and performance in minor crops. ► This is the first report for the determination of spinetoram and its metabolites using tandem mass in minor crops. 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 0.03mg/kg for all the tested analytes in amaranth and parsley, respectively. Recovery values, at spiking levels 0.05 and 0.25mg/kg, ranged from 71.0% to 115.2% with relative standard deviations