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Hyo-Min Heo,Hyeong-WookJo,Kyu-Won Hwang,Jung-Hun Sun,Joon-Kwan Moon 한국농약과학회 2021 한국농약과학회 학술발표대회 논문집 Vol.2021 No.11
Simultaneous analytical method using LC/MSMS for imidazolinone herbicides from livestock (egg, milk, beef, pork and chicken) for monitoring was developed with QuEChERS preparation. Sample weighing (5g) in a 50mL conical tube, added 0.1 M potassium phosphate dibasic solution (5mL) was shaken for 10min. After 0.5mL 6 NHCl, 10mL acetonitrile were added, it was shaken for 10min. And QuEChERS extraction salt (Original method, 4g MgSO₄, 1g NaCl) were added to the sample in the 50 mL conical tube. The mixture was strongly shaken for 1 min and was centrifuged at 3,000g for 10 min. The acetonitrile layer was purification with dSPE (150mg MgSO₄, 25mg C18) and was centrifuged at 13,000g for 5min. The supernatant was filtered with a membrane filters (pore size: 0.2um) before analysis. ME (%, Matrix effect) for almost analytes range were -6.56 to 5.70%. MLOD (Method LOD) and MLOQ (Method LOQ) was calculated by S/N ratio. MLOQs were 0.01 mg/kg. The linear correlation coefficients (r2) were > 0.99 within the range of 2 ~ 100 ug/kg for all of the 3 imidazolinone herbicides. The percentages (of imidazolinone herbicides) recovers were in the range of 84.1 ~ 110.6% (0.01mg/kg level), 90.8 ~ 97.1% (0.1mg/kg level) and 94.4 ~ 102.1% (0.5mg/kg level) within the validation criteria (recover; 70-120% with RSD < 20%)
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