• Analytical Science and Technology
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• v.29 no.4
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• pp.179-185
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• 2016

An effective analytical method has been developed for the determination of β-blockers(atenolol, metoprolol and propranolol) and 6 β-lactams(amoxicillin, penicillin G, cefaclor, cefadroxil, cephalexin and cephradine) in water samples using two different cartridges. The samples were extracted by solid-phase extraction (SPE) with the usage of polymeric hydrophile-lipophile balance(HLB cartridges) and strong cation-exchange mixed-mode polymeric sorbent (MCX cartridges). A XDB-C₁₈ column(1.8 μm; 3.0 mm × 100 mm) was used for the sufficient chromatographic resolution. The calibration curves showed good linearity with high correlation coefficients (>0.995). The method detection limits (MDL) and the limits of quantification(LOQ) were from 1.1 to 3.9 ng/L and from 5 to 13 ng/L, respectively. The method was applied for the determination of the target compounds in tributaries and raw water of the Han River and these were found at N.D. to 0.209 μg/L.

• Journal of fish pathology
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• v.10 no.2
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• pp.125-135
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• 1997

The possibility of identification of families of antibacterial agent residues in fish tissue was studied by disk assay using three test organisms, Bacillus subtilis BGA, Micrococcus luteus ATCC 9341, and Bacillus cereus var. mycoides ATCC 11778. In the present method, a simple clean-up procedure was performed to obtain the aqueous solution from homogenized flounder muscle sample(10g) in Mcilvaine buffer. Then, aqueous solution was fractionated into A and B to be used in disk assay by choloroform and Sep-Pak $C_{18}$ cartridge column after being defatted in hexane. The chloroform layer of fraction A was used for the analysis of macrolide antibiotics(ML), sulfa drugs(SA), chloramphenicol(CP), and quinolone antibiotics(QN). Adsorbed materials to Sep-Pak $C_{18}$ of fraction B were also employed for the analysis of penicillins(PC), tetracyclines(TC), and nitrofuran derivatives(NF) Minimun-detectable concentrations by the present method were, $0.1{\mu}g$/g for oxytetracycline, tetracycline, doxycycline, spiramycin and ciprofloxacin, $0.025{\mu}g$/g for erythromycin and ampicillin, $1.0{\mu}g$/g for sodium nifurstyrenate and florfenical, $0.25{\mu}g$/g for sulfamonomethoxie and sulfadimethoxine, $2.5{\mu}g$/g for oxolinic acid and flumequine, and $15{\mu}g$/g for piromidic acid, respectively. Three test organisms showed different sensitivity patterns for each family of antibacterial agent. Sensitivity patterns were B. cereus > B. subtilis > M. luteus for TC and NF, M. luteus > B, subtilis > B. cereus for ML and PC, B. cereus = B. subtilis > M. luteus for CP and QN, and B. subtilis > B. cereus＝M. luteus for SA. The present method utilizing these characteristics could be useful as a routine screening test for the determination of family of antibacterial agent residues in fish tissue.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.30-39
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• 2019

An analytical method was developed for the determination of sedaxane in agricultural products using liquid chromatograph-tandem mass spectrometry (LC-MS/MS). The samples were extracted with acetonitrile and partitioned with dichloromethane to remove the interference, and then purified by using silica SPE cartridges to clean up. The analytes were quantified and confirmed by using LC-MS/MS in positive ion mode using multiple reaction monitoring (MRM). The matrix-matched calibration curves were linear over the calibration ranges ($0.001-0.25{\mu}g/mL$) into a blank extract with $r^2$>0.99. For validation, recovery tests were carried out at three different concentration levels (LOQ, 10LOQ, and 50LOQ, n=5) with five replicates performed at each level. The recoveries were ranged between 74.5 to 100.8% with relative standard deviations (RSDs) of less than 12.1% for all analytes. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL 40, 2003) and Food Safety Evaluation Department guidelines (2016). The proposed analytical method was accurate, effective and sensitive for sedaxane determination in agricultural commodities.