• KSBB Journal
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• v.11 no.5
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• pp.606-612
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• 1996

A specific ammino auid in a mixture can be crystallized inside an ion exchange column when displacer concentration is high enough to concentrate the amino acid in a pure band beyond its solubility limit. Glutamic acid formpd a discrete crystal layer in a cation exchanger column by operating displacement development mode and using a high concentration of displacer NaOH. The glutamic acid crystal formed was eluded from the column with the effluent stream and collected in a fraction collector. When 1.0 M of NaOH was used as a displacer, more than 60% of the loaded glutamic acid was recovered as crystal. The continuous crystallization and dissolution of crystal occurred, resulting in apparent movement of the crystal along the column without clogging or pressure increase. NaOH was proved a better displacer than NaCl because hydroxide ions neutralized hydrogen ions released from the resin and thus reduced the number of hydrogen ion competing with sodium ion for re-adsorption. The displacement development process coupled with crystallization provided higher concentration and recovery of glutamic acrid than conventional chromatography.

• The Korean Journal of Pesticide Science
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• v.16 no.3
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• pp.202-208
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• 2012

A high-performance liquid chromatographic (HPLC) method was developed to determine residues of cyromazine, a triazine insecticide, in agricultural commodities. Cyromazine was extracted with 90% aqueous methanol from representative crops which comprised brown rice, oyster mushroom, oriental melon, watermelon, and Chinese cabbage. Following to evaporation of methanol in the extract, the aqueous concentrate was acidified to form the protonated cyromazine. Dichloromethane partition was then applied to remove nonpolar co-extractives in the aqueous phase. Strong cation-exchange chromatography using Dowex 50W-X4 resin was employed for final purification of the extract. Cyromazine was successfully separated on a Zorbax SB-Aq $C_{18}$ column showing high retention for polar compounds. Cyromazine was sensitively quantitated by ultraviolet absorption at 214 nm. Limit of quantitation (LOQ) of the method was 0.04 mg/kg irrespective of sample types. Each crops were fortified at 3 different concentrations of cyromazine for recovery test. Mean recoveries from samples fortified at LOQ~2.0 mg/kg in triplicate ranged 80.2~103.3% in five agricultural commodities. Relative standard deviations in recoveries were all less than 6%. A selected-ion monitoring LC/MS method with electrospray ionization in positive-ion mode was also provided to confirm the suspected residue. The proposed method was reproducible and sensitive enough to routinely determine and inspect the residue of cyromazine in agricultural commodities.