• 한국물환경학회지
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• 제32권6호
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• pp.628-648
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• 2016

Increased attention has been paid to the presence of veterinary antibiotics in various environmental matrices due to their toxicological behavior in the ecosystem and development of antibiotic-resistant strains of pathogenic bacteria. In the this review, 37 target antimicrobials were selected based on annual sales of antibiotics for livestock in South Korea 2014. Also, extraction and clean-up methods for the determination of the antibiotic residues in liquid samples including water, milk, and honey were comprehensively reviewed in the literature. Solid-phase extraction (SPE) was commonly used as a pre-treatment method for the samples. Most of the analytes were extracted in acidic conditions (2.5~4.0) except for aminoglycosides, which were extracted in neutral conditions (7.0~8.0). ${\beta}-Lactams$ showed the highest recoveries in neutral pH due to their degradation characteristics in acidic media. Starta-X, Oasis HLB, and Oasis MCX were frequently applied as an SPE cartridge and Oasis HLB showed the highest recoveries for the majority of antibiotic classes. The homogenized honey and milk were extracted by mixing with acids for deproteinization. Solids and other interfering substances in the extract were eliminated by centrifugation followed by membrane filtration or SPE before injection into HPLC.

• Journal of Microbiology and Biotechnology
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• 제14권2호
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• pp.256-261
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• 2004

In order to detect chitooligosaccharides (COS) in soybean paste, tandem immunoaffinity chromatography and enzyme-linked immunosorbent assay (ELISA) were developed. Polyclonal anti-chitooligosaccharides mixture (CaSM) antibody specific to COSM was attached to Sepharose gel for initial sample cleanup and concentration of COS in soybean paste. COS was eluted and quantified by competitive direct ELISA (cdELISA). Average ELISA recoveries from the column using binding buffer spiked with COSM at levels of 0.5, 2.0, 5.0, and $10.0\mu$g/ml were 79.8, 72.0, 77.7, and 60.6%, respectively, with a mean recovery of 72.5%. Mean inter-well and inter-assay coefficients of variation (CV) were 7.7% and 10.3%, respectively. Average recoveries from soybean paste spiked with COSM at levels of 2, 6, 20, and $60\mu$g/g were 115, 91.7, 91, and 73.3%, respectively, with a mean recovery of 92.8%. Mean inter-well and inter-assay CV were 12.9% and 16%, respectively. The COS was detected from 24 out of 25 homemade Korean soybean paste samples at an average of $14.0\mu$g/g (n, 25; range, $0-51.2 \mu$g/g) and from 13 out of 14 commercially made soybean paste samples at an average of $4.1\mu$g/g(n, 14; range, $0-18.4\mu$g/g). The tandem immunoaffinity chromatography-cdELISA that was developed in this study showed that the level of COS eluted from homemade soybean paste was higher than that of the commercially made ones. In addition, the level of COS eluted from commercially available soybean paste in Korea was higher than that of the ones in Japan.

• 한국물환경학회지
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• 제22권5호
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• pp.879-886
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• 2006

The analytical methods of polychlorinated dibenzo-p-dioxins, polychlorinated dibenzofurans (PCDD/Fs) for water sample with extremely low concentration was developed to extract large volume and to improve fast chromatography for clean up. Semi-automated solid phase extraction (SPE) system and column coupling chromatography using elution pump was optimized and applied to each processes of treatment plant. Results of disk type SPE indicated that this system was applicable below 40 L of aqueous sample with a flow rate of 0.08 ~ 0.2 L/min. Average recoveries of SPE using labeled sampling spike of $^{37}Cl$-2,3,7,8-TCDD was 97%. Column coupling method resulted in reduced clean up time, solvent volume, increased average recoveries with constant elution rate. The combined methods were applied to the monitoring of drinking water treatment plant. Limits of detection (LOD) of each process were calculated. For example, LOD of raw and treated water ranged 0.094~0.968 pg/L and 0.028~0.364 pg/L, respectively. Combined methods of extraction and cleanup techniques provided fast analysis of PCDD/Fs with high accuracy and low LODs for water samples.

• 분석과학
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• 제10권6호
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• pp.395-402
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• 1997

시료의 매질에 따른 추출법의 문제점과 사용 가능성을 조사하기 위해 환경처 발행의 폐기물공정시험방법과 EPA 3050법을 비교 연구하였다. 이를 위해 sludge와 개펄 시료에 12종의 무기 priority pollutants(Cd, Cr, Cu, Pb, Ni, Zn, As, Sb, Se, Hg, Be, Tl)를 첨가하여 분석용 시료를 조제하고 AAS, HG-AAS, 그리고 ICP/MS를 사용하여 각 추출방법에 대한 대상 원소의 회수율, 상대표준편차 및 method detection limit를 측정하었다. EPA 3050법에 따라 추출한 경우 회수율이 좋지 않은 As, Sb, Se를 제외한 평균 회수율은 93%였다. 그러나 폐기물공정시험방법의 용출시험방법으로 실험한 경우는 전반적으로 회수율이 32%로 매우 좋지 않을 뿐만 아니라 시료의 매질에 의한 영향을 심각하게 받는 것으로 조사되었다.

• 분석과학
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• 제23권4호
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• pp.405-413
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• 2010

축산물(소의 근육 및 간)중에 잔류하는 합성 글루코코티코이드 6종 (betamethasone, dexamethasone, prednisone, prednisolone, methylprednisolone, flumethasone)에 대한 동시분석방법을 확립하였다. 효과적인 기기분석을 위해서 시료는 C18 고체상 카트리지를 사용하여 에틸아세테이트 용매를 사용하여 추출/정제하였다. C18 컬럼을 사용하여 분리한 후 음이온 전기분무 질량분석법의 multiple reaction monitoring 방법을 사용하여 정량 및 정성 분석을 수행하였다. 효과적이고 감도있는 HPLC-MS/MS 분석을 위해서 0.1% 포름산이 포함된 물과 아세토나이트릴이 이동상 용매로 사용되었다. 메트릭스와 약물의 종류에 따라서 검출한계(LOD)는 $0.2-0.1\;{\mu}g$/kg, 정량한계(LOQ)는 $0.8-3.4{\mu}g$/kg 이었으며, 회수율은 89.5-119.6%이었다. 확립된 기존의 방법들에 비해 6종의 글루코코티코이드의 동시분석 방법이 간소화되었고, 좋은 정확도, 정밀도 및 회수율을 나타내었으며, 축산 육류 중에 잔류하는 글루코코티코이드들 분석하는데 사용될 수 있을 것이다.

• 한국식품과학회지
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• 제47권3호
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• pp.401-404
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• 2015

가공식품 중 돈육의 검출을 위한 샌드위치 ELISA (sELISA)의 조건을 확립하기 위해 항돼지IgG 항체(goat anti-pig IgG antibody)를 이용하였다. 이때, 돈육의 검출범위는 $3-1,000ppm({\mu}g/mL)$이며, 검출한계는 2 ppm이었다. 특이항체의 교차반응 결과, 돼지IgG에 대한 반응성을 100%로 하였을 때, 돈육에 대한 반응성은 0.18%로 나타났으나, 여타의 식품원료에 대하여 반응하지 않았다. 열처리한 돈육에 대한 항체의 반응성은 $70^{\circ}C$까지는 32% 이상으로 양호하였으나 $80^{\circ}C$ 이상에서는 0.11% 이하로 반응성 급격히 감소하였다. 크림스프, 이유식, 어묵, 소스에 대한 spike test에서 돈육의 분석회수율은 각각 8.8, 45, 36, 39%로 나타났다. sELISA에 의하여 12점의 시판 가공식품 시료 중 돈육의 함유 유무를 조사한 결과, 정성적으로 원료의 표시사항과 100% 일치하였다.

• Bulletin of the Korean Chemical Society
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• 제25권3호
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• pp.365-372
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• 2004

Two simple, rapid and sensitive spectrophotometric methods for the determination of three fluoroquinolones, namely levofloxacin, norfloxacin and ciprofloxacin have been performed either in pure form or in their tablets. In the first method, levofloxacin and norfloxacin are directly treated with bromocresol green (BCG) in dichloromethane while ciprofloxacin is allowed to react with the same dye in aqueous acidic buffer. Highly yellow colored complex species were formed instantaneously in case of levofloxacin and norfloxacin or after extraction into dichloromethane for ciprofloxacin. The formed complexes are quantified spectrophotometrically at their absorption maxima at 411 nm for levofloxacin and 412 nm for norfloxacin and ciprofloxacin. The second method involves the reaction of levofloxacin with ${\rho}$-chloranilic acid ( ${\rho}$-CA) and norfloxacin with tetracyanoethylene (TCNE) in acetonitrile to give complexes with maximum absorbance at 521 and 333 nm for the two drugs, respectively. Adopting the first procedure, calibration graphs were linear over the range 1- 20 ${\mu}g\;mL^{-1}$ with mean percentage recoveries of 100.41 ${\pm}$ 0.72, 99.99 ${\pm}$ 0.54 and 100.23 ${\pm}$ 0.91 for the theree drugs, respectively. For the second procedure, the concentration ranges were 15-250 ${\mu}g\;mL^{-1}$ for levofloxacin using ${\rho}$-CA and 0.8-16 ${\mu}g\;mL^{-1}$ for norfloxacin using TCNE with mean percentage recoveries of 99.88 ${\pm}$ 0.45 and 100.26 ${\pm}$ 0.68 for the two drugs, respectively. The proposed methods were successfully applied to determine these drugs in their tablet formulations and the results compared favorably to that of reference methods. The proposed methods are recommended for quality control and routine analysis.

• 한국동물위생학회지
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• 제34권4호
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• pp.429-439
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• 2011

This article described the comparison of a quick, easy, cheap, effective, rugged and safe (QuEChERS) sample preparation and the classical method established by National Veterinary Research and Quarantine Service (NVRQS) for the determination of pesticide residues in livestock products using GC-tandem mass spectrometry. The classical method by NVRQS used liquid-liquid partioning followed by evaporizing. The modified QuEChERS entailed extraction of 2 g sample with 15 ml acetonitrile containing 1% acetic acid followed by addition of 6 g anhydrous magnesium sulfate and 1.5 g sodium acetate. After centrifugation, 6 ml of the extract underwent a cleanup step (in a technique known as column-based solid phase extraction) using 400 mg each of $C_{18}$ and primary secondary amine sorbents plus 1,200 mg magnesium sulfate. The quantitation of individual pesticides by both methods was based on tissue standard calibration curves with a correlation coefficient in excess of 0.98 for the 24 pesticides. The detection limits by the classical method were ranged 1.3~5.0 ${\mu}g$/kg, with mean recoveries between 76.2% and 114.3% except aldrin (59.3%) and deltamethrin (63.6%). The detection limits by modified QuEChERS were ranged 0.3~6.2 ${\mu}g$/kg, with mean recoveries between 68.0% and 114.3% except dimethipin (152.6%), chlorfenvinphos (138.1%), 4,4-DDT (61.5%), aldrin (60.4%) and chinomethionate (30.3%).

• Bulletin of the Korean Chemical Society
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• 제27권1호
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• pp.77-81
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• 2006

The commercially available Amberlite XAD-2 and XAD-4 resins were modified with macrocyclic protoporphyrin IX (PPIX) or tetrakis(p-carboxyphenyl) porphyrin (TCPP) to enhance the adsorption capacity for phenol and chlorophenols. The chemically modified polymeric adsorbents (XAD-2+PPIX, XAD-2+TCPP, XAD-4+PPIX, and XAD-4+TCPP) were applied to the solid phase extraction as an adsorbent material for the preconcentration of phenol and chlorophenols in environmental waters. Generally, the synthesized adsorbents showed higher recoveries than underivatized adsorbents, XAD-2 and XAD-4, without matrix interferences. Especially, XAD-4+PPIX showed more than 90% recoveries for all compounds used in this study including hydrophilic phenol. The major factor for the increase of the adsorption capacity was the increase of $\pi$-$\pi$ interaction between adsorbents and samples due to the introduction of the porphyrin molecule. However, the breakthrough volumes and recovery values of the XADs+TCPP columns were slightly decreased for the bulky chlorophenols such as TCP and PCP. Using molecular mechanics methods, the structures of TCPP and PPIX were compared with that of porphine, the parent molecule of porphyrin. Four bulky p-carboxyphenyl groups of TCPP were torsional each other, thus the molecular plane of TCPP were not on the same level. In conclusion, the decrease of breakthrough volumes and recovery values of XADs+TCPP columns for bulky phenols can be explained by the steric hindrance of the $\pi$-$\pi$ interaction between porphyrin plane and the phenols.

• 한국작물학회지
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• 제47권2호
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• pp.132-136
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• 2002

The rice straw managements are essential for maintaining soil fertility as well as reducing chemical fertilizer application in paddy field. A field experiment was conducted on moderately well draining alluvial paddy soil to investigate the decomposition pattern of rice straw. The mesh bags containing the rice straw harvested in the previous year were placed at soil surface and buried into around 10cm depth and recovered periodically for determining the straw decomposition. Pot experiments were conducted to investigate the fates of N released from $^{15}$ N-labeled rice straw under different levels of N fertilizer application. The overall decomposition patterns of rice straw were similar for the two incorporation depths in transplanted paddy field. The straw incorporated at transplanting date showed weight loss of about 50%, 70% and 90% after 2 months, 5 months, and 2 years, respectively. The decompositions of straw cell wall components showed somewhat different pattern. The decompositions of cellulose and silica were similar to that of dry weight while the decomposition of lignin was slower than that of cellulose and silica. N was released from rice straw 42% and 65 % of the initial N after one month and after five months, respectively. P release was faster than N release. Recoveries of rice straw-$^{15}$ N by rice plants were 10.2, 13.4 and 14.9% in 0, 120 and 240 mg N pot$^{-1}$ , respectively. Soil recoveries of rice straw $^{15}$ N were 17.3, 20.6 and 18.9% in 0, 120 and 240mg N pot$^{-1}$ , respectively.