期刊
ANALYTICA CHIMICA ACTA
卷 702, 期 1, 页码 127-135出版社
ELSEVIER SCIENCE BV
DOI: 10.1016/j.aca.2011.06.034
关键词
Enantioselective gas chromatographic separation; Simeconazole; Quick, easy, cheap, effective, rugged and safe; Solid-phase extraction; Gas chromatography/ion trap mass spectrometry
资金
- Nature Science Foundation of China (NSFC) [31071706]
- foundation of the National Basic Research Program of China (The 973 Program) [2009CB119000]
- Public Service Sector Research and Development Project [200903054, 200903033]
A rapid and effective method for enantioselective determination of simeconazole enantiomers in food products (cucumber, tomato, apple, pear, wheat and rice) has been developed. The enantiomers were resolved by capillary gas chromatography (GC) using a commercial chiral column (BGB-172) and a temperature program from 150 degrees C (held for 1 min) and then raised at 10 degrees C min(-1) to 240 degrees C (held for 10 min). This enantioselective gas chromatographic separation was combined with a clean-up/enrichment procedure based on the modification of QuEChERS (quick, easy, cheap, effective, rugged and safe) method. Co-extractives were removed with graphitized carbon black/primary secondary amine (GCB/PSA) solidphase extraction (SPE) cartridges using acetonitrile: toluene (3:1, v/v) as eluent. Gas chromatography/ion trap mass spectrometry (GC-ITMS) with electron ionization (El) was then used for qualitative and quantitative determination of the simeconazole enantiomers. Two precursor-to-product ion transitions (m/z 121-101 and 195-153) with the best signal intensity were chosen to build the multiple-reaction monitoring (MRM) acquisition method. The limits of detection for each enantiomer of simeconazole in six food products ranged between 0.4 and 0.9 mu g kg(-1), which were much lower than maximum residue levels (MRLs) established by Japan. The methodology was successfully applied for the enantioselective analysis of simeconazole enantiomers in real samples, indicating its efficacy in investigating the environmental stereochemistry of simeconazole in food matrix. (C) 2011 Elsevier B.V. All rights reserved.
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