Determination of spinetoram and its metabolites in ...

9 downloads 13636 Views 1MB Size Report
Apr 21, 2012 - quick, easy, cheap, effective, rugged, and safe (QuEChERS)-based extraction. Afterwards .... either the public or private sectors, and (5) feature plant breeding ... pesticide manufacturers to obtain registration of pesticides for.
Food Chemistry 134 (2012) 2552–2559

Contents lists available at SciVerse ScienceDirect

Food Chemistry journal homepage: www.elsevier.com/locate/foodchem

Analytical Methods

Determination of spinetoram and its metabolites in amaranth and parsley using QuEChERS-based extraction and liquid chromatography–tandem mass spectrometry Ki Hun Park a,1, Jeong-Heui Choi a,1, A.M. Abd El-Aty b,⇑, 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,⇑ a

Natural Products Chemistry Laboratory, College of Agriculture and Life Science, Chonnam National University, 77 Yongbong-ro, Buk-gu, Gwangju 500-757, Republic of Korea Department of Pharmacology, Faculty of Veterinary Medicine, Cairo University, 12211 Giza, Egypt National Agricultural Products Quality Management Service, Products Safety Inspection Laboratory, Gwangsan-Gu, Gwangju, Republic of Korea d Pesticide Safety Division, National Institute of Agriculture Science and Technology, Rural Development Administration, Suwon 441-707, Republic of Korea b c

a r t i c l e

i n f o

Article history: Received 12 October 2011 Received in revised form 22 February 2012 Accepted 16 April 2012 Available online 21 April 2012 Keywords: Simultaneous determination Spinetoram Metabolites Minor crops LC–ESI–MS/MS

a b s t r a c t 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