• The Korean Journal of Pesticide Science
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• v.19 no.1
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• pp.5-13
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• 2015

A chromatographic method for the determination of imazapyr, a non-selective herbicide, in agricultural commodities was developed to use safety control of pesticide residue on crops, and was fully validated as an official method for residue analysis. Agricultural commodities, mandarin (fruit), hulled rice (cereal grains), pepper (vegetables), potato (potatoes) and soybean (beans) were extracted with methanol and partitioned with dichloromethane to remove the interference obtained from sample extracts, adjusting pH to 2.5 by 4N hydrochloric acid. Finally, they were analyzed by high performance liquid chromatography coupled to UV detector (HPLC-UVD). The developed method had the linearity in the range of test concentrations with coefficients of determination ($r^2$) more than 0.99. Recovery studies were carried out at three concentration levels (LOQ, 10LOQ, and 50LOQ) performing five replicates at each level. Recoveries were ranged between 72.1 to 108.0%, with relative standard deviations less than 10%. A consistent recovery was determined according to the CODEX guidelines (CAC/GL40, 2003). Finally, LC/MS with selected ion monitoring was also applied to confirm the suspected residues of imazapyr in agricultural samples. This developed method for determination of imazapyr residues in agricultural commodities. can be used as an official method.

• Food Science and Preservation
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• v.17 no.5
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• pp.741-751
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• 2010

We evaluated the nutritional value of a Monascus pilosus mycelial ethanolic extract (MEM) and culture filtrate (CFM) by determining the contents of monacolin K and citrinin, and by measuring antioxidant and antimicrobial activities. The yields of freeze-dried MEM and CFM powder were 4.02% and 3.35% of wet weight, respectively. Pigment content ($OD_{500}$ value) of MEM (0.79) and CFM (0.63) were lower than those of commercial rice beni-koji ethanolic extracts (EERB) (0.87), but were in good agreement with the L*, a*, and b* values and the hue angles of the products. The total monacolin K content of MEM (24.91 mg%) was higher than those of CFM (1.27 mg%) and EERB (14.65 mg%). However, the active monacolin K content of EERB (5.48 mg%) was higher than those of MEM (3.35 mg%) and CFM (0.4 mg%). Citrinin was not detected in any sample. The total polyphenol content of MEM (4.68%, w/w) was similar to that of CFM (4.29%, w/w), thus 13.75.20.94% higher than that of EERB. The total flavonoid content of EERB was 6.8.7.0-fold higher than those of MEM (0.64%, w/w) and CFM (0.66%, w/w). The total antioxidant capacity of CFM (3.51%, w/w) was 1.62.2.08-fold higher than those of MEM (2.74%, w/w) and EERB (1.69%, w/w). The electron-donating capacities of 1% (w/v) solutions of CFM, MEM, BHT, and EERB were 86.20%, 77.25%, 77.25%, and 44.82%, respectively, and the corresponding reducing powers ($OD_{700}$ values) were 2.1, 2.4, 1.1, and 1.6, respectively. SOD(superoxide dismutase)-like activities were in the order MEM (39.85%) > BHT (37.68%) > EERB (26.70%) > CFM (21.5%). Although the TBARS (% value) of MEM was a little lower than that of BHT, it was higher than those of CFM and EERB. The antibacterial activities of CFM acting on Bacillus brevis and Escherichia coli were somewhat higher than those of MEM, whereas the activities of MEM on Bacillus subtilis, Listeria monocytogenes, Staphylococcus aureus, Staphylococcus epidermidis, and Salmonella enteritidis were higher than those of CFM. However, the antibacterial activities of MEM and CFM were less than those of EERB and BHT. In conclusion, although further studies are needed, we offer experimental evidence that the by-products of M. pilosus MEM and CFM contain significant antioxidant and antimicrobial activities that may be useful in the development of healthy foods.

• Journal of Food Hygiene and Safety
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• v.36 no.3
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• pp.228-238
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• 2021

The aim of this research was to develop a rapid and easy multi-residue method for determining dimethipin, omethoate, dimethipin, chlorfenvinphos and azinphos-methyl in agricultural products (hulled rice, potato, soybean, mandarin and green pepper). Samples were prepared using QuEChERS (Quick, Easy, Cheap, Effective, Rugged and Safe) and analyzed using gas chromatography-tandem mass spectrometry (GC-MS/MS). Residual pesticides were extracted with 1% acetic acid in acetonitrile followed by addition of anhydrous magnesium sulfate (MgSO₄) and anhydrous sodium acetate. The extracts were cleaned up using MgSO₄, primary secondary amine (PSA) and octadecyl (C₁₈). The linearity of the calibration curves, which waas excellent by matrix-matched standards, ranged from 0.005 mg/kg to 0.3 mg/kg and yielded the coefficients of determination (R²) ≥ 0.9934 for all analytes. Average recoveries spiked at three levels (0.01, 0.1, 0.5 mg/kg) and were in the range of 74.2-119.3%, while standard deviation values were less than 14.6%, which is below the Codex guideline (CODEX CAC/GL 40).