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식품의약품안전처 SESSION : GC-MS/MS를 이용한 현미 중 112 잔류농약의 다성분 동시 분석
Simultaneous Analysis of 112 Pesticide Multi-Residues in Rice by GC-MS/MS
이종화 ( Jong Hwa Lee ) , 차경훈 ( Kyung Hoon Cha ) , 이진범 ( Jin Beum Lee ) , 김병준 ( Byung Joon Kim ) , 이혜리 ( Hyeri Lee ) , 김은혜 ( Eun Hye Kim ) , 김수희 ( Su Hee Kim ) , 김정한 ( Jeong Han Kim )
UCI I410-ECN-0102-2015-500-000630157
This article is 4 pages or less.

A multi-residue method for simultaneous analysis of 112 pesticides by GC-MS/MS (gas chromatography-tandem triple quadrupole mass spectrometry) in rice was developed. Three sample preparation methods such as QuEChERS (quick, easy, cheap, effective, rugged and safe), KFDA method and PLS (Japanese positive list system method) were applied to rice for analysis pesticide. Recovery, matrix effect and process efficiency of the sample preparation methods were compared. For GC-MS/MS, two MRM (multiple reaction monitoring) transitions per compound were optimized to increase confidence in identification. Correlation coefficients (R2) of calibration curves and LOQ (limit of quantitation) were in range >0.99 and 0.001-0.050 mg kg-1, respectively. Quantitation was determined using matrix matched calibration curves at concentration ranging from 0.002 mg kg-1 to 0.2 mg kg-1. To evaluate performance of the each sample preparation method, recovery tests were carried out on rice at spiking levels 0.01 and 0.05 mg kg-1. A most of compounds could be recovered with QuEChERS method as well as with the PLS method, while the KFDA method could not recover 10 pesticides. Average recovery in the range of 70-120% (RSD ≤20%) at the lower fortification level of 0.01 mg kg-1 were approximately 91.1% (QuEChERS), 89.3% (KFDA method) and 83.0% (PLS method) of 112 compounds. At higher fortification levels of 0.05 mg kg-1, approximately 99.1% (QuEChERS), 45.5% (KFDA method) and 93.8% (PLS method) of 112pesticides were in the range of 70-120% (RSD ≤20%) which is a validation criteria of European Union in single residue analysis. The QuEChERS method was found to produce least matrix effect while the KFDA method produced highest. In aspect on process efficiency, the QuEChERS method demonstrated the advantage of less-time, less-reagents, and less-labor consuming in sample preparation procedure, and gave best recovery rates.

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