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KMID : 0881720190340020124
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Journal of Food Hygiene and Safety
2019 Volume.34 No. 2 p.124 ~ p.134
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Development of a Simultaneous Analytical Method for Determination of Insecticide Broflanilide and Its Metabolite Residues in Agricultural Products Using LC-MS/MS
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Park Ji-Su
Do Jung-Ah
Lee Han-Sol
Park Shin-Min
Cho Sung-Min
Kim Ji-Young
Shin Hye-Sun
Jang Dong-Eun
Jung Yong-Hyun
Lee Kang-Bong
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Abstract
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An analytical method was developed for the determination of broflanilide and its metabolites in agri- cultural products. Sample preparation was conducted using the QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) method and LC-MS/MS (liquid chromatograph-tandem mass spectrometer). The analytes were extracted with ace- tonitrile and cleaned up using d-SPE (dispersive solid phase extraction) sorbents such as anhydrous magnesium sulfate, primary secondary amine (PSA) and octadecyl (C18). The limit of detection (LOD) and quantification (LOQ) were 0.004 and 0.01 mg/kg, respectively. The recovery results for broflanilide, DM-8007 and S(PFP-OH)-8007 ranged between 90.7 to 113.7%, 88.2 to 109.7% and 79.8 to 97.8% at different concentration levels (LOQ, 10LOQ, 50LOQ) with relative stan- dard deviation (RSD) less than 8.8%. The inter-laboratory study recovery results for broflanilide and DM-8007 and S (PFP-OH)-8007 ranged between 86.3 to 109.1%, 87.8 to 109.7% and 78.8 to 102.1%, and RSD values were also below 21%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40-1993, 2003) and the Food and Drug Safety Evaluation guidelines (2016). Therefore, the proposed analytical method was accurate, effec- tive and sensitive for broflanilide determination in agricultural commodities.
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KEYWORD
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Broflanilide, LC-MS/MS, Insecticide, Analytical method, Agricultural products
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