Analysis of kresoxim-methyl and its thermolabile metabolites in Korean plum: An application of pepper leaf matrix as a protectant for GC amenable metabolites


Rahman M. M., Park J., HASSIBELNABY A. M. A., Choi J., Cho S., Yang A., ...Daha Fazla

JOURNAL OF SEPARATION SCIENCE, cilt.36, sa.1, ss.203-211, 2013 (SCI-Expanded) identifier identifier identifier

  • Yayın Türü: Makale / Tam Makale
  • Cilt numarası: 36 Sayı: 1
  • Basım Tarihi: 2013
  • Doi Numarası: 10.1002/jssc.201200618
  • Dergi Adı: JOURNAL OF SEPARATION SCIENCE
  • Derginin Tarandığı İndeksler: Science Citation Index Expanded (SCI-EXPANDED), Scopus
  • Sayfa Sayıları: ss.203-211
  • Atatürk Üniversitesi Adresli: Hayır

Özet

A new method was developed for kresoxim-methyl (parent compound) and its two thermolabile metabolites, BF 490-2 and BF 490-9, in Korean plum, introducing pepper leaf matrix as a natural analyte protectant for GC-amenable metabolites using a GC-electron capture detector. Samples were extracted with a simple and rapid method using a mixture of ethyl acetate-n-hexane (1: 1) and salts, and purified via SPE. Due to the elution gap between parent compound and metabolites in the SPE cartridge and matrix interference, kresoxim-methyl was isolated separately from its metabolites. An optimized amount of pepper leaf matrix (0.25 g/mL) was added to the metabolites prior to each injection. Calibration curves were linear over the concentration ranges with coefficient of determination (r(2)) >= 0.999. The method was validated in triplicate at two fortification levels, giving recoveries ranging between 74.3 and 101.4%, and RSDs less than 5%. The LOD and LOQ were 0.015 and 0.05 mg/kg, respectively. The method was successfully applied to real samples where kresoxim-methyl residues were detected in field-incurred plum samples. Residues were confirmed using GC-MS.