• Bulletin of the Korean Chemical Society
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• 제20권6호
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• pp.696-700
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• 1999

A method has been developed for the determination of trace anion impurities in concentrated hydrogen peroxide. The method involves on-line decomposition of hydrogen peroxide, ion chromatographic separation and subsequent suppressed-type conductivity detection. H2O2 is decomposed in Pt-catalyst filled Gore-Tex membrane tubing and the resulting aqueous solution containing analytes is introduced to the injection valve of an ion chromatograph for periodic determinations. The oxygen gas evolving within the membrane tubing escapes freely through the membrane wall causing no problem in ion chromatographic analysis. Decomposition efficiency is above 99.99% at a flow rate of 0.4mL/min for a 30% hydrogen peroxide concentration. Analytes are quantitatively retained. The analysis results for several brands of commercial hydrogen peroxides are reported.

• 분석과학
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• 제33권1호
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• pp.42-48
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• 2020

Bromate is a disinfection by-product generated mainly from the oxidation of bromide during the ozonation and disinfection process in order to remove pathogenic microorganism of drinking water, and classified as a possible human carcinogen by International Agency for Research of Cancer (IARC) and World Health Organization (WHO). For the purpose of determining the trace level concentration of bromate, several sensitive techniques are applied mostly based on suppressed conductivity detection and UV/Visible detection after postcolumn reaction (PCR). In this study, the suppressed conductivity detection method and the PCR-UV/Visible detection method through the triiodide reaction were compared to analyze the trace bromate in water samples and estimated for the availability of these analytical methods. In addtion, the state-of-the-art techniques was applied for the determination of trace level bromate in various water matrices, i.e., soft drinking water, hard drinking water, mineral water, swimming pool water, and raw water. In comparison of two analytical methods, it was found that the conductivity detection had the suitable advantage to simultaneously analyze bromate and inorganic anions, however, the bromate might not be precisely quantified due to the matrix effect especially by chloride ion. On the other hand, the trace bromate was analyzed effectively by the method of PCR-UV/Visible detection through triiodide reaction to satisfactorily minimize the matrix interference of chloride ion in various water samples, showing the good linearity and reproducibility. Furthermore, the method detection limit (MDL) and recovery were 0.161 ㎍/L and 101.0-108.1 %, respectively, with a better availability compared to conductivity detection.

• 환경위생공학
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• 제21권4호
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• pp.29-38
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• 2006

This study included the development of analytical method for determining perchlorate in water sample. The analytical condition was referred in EPA 314.0 method which use ion chromatography and the concentrator column was replaced by the guard column. Concentrating 10mL raw or treated water sample on to AGl6 guard column made it possible to get the LOD(Limit of Detection) of $0.73\;{\mu}g/L$. The total run time was 11 minutes and during run time next sample could be concentrated on AGl6 guard column. Compared to the Concentration method which needed manual operation, the Direct Injection method could screen the many water samples. The LOD of the Direct Injection method was higher and the sensitivity was lower than that of the Concentration method. The RSDs(Relative Standard Deviations) were lower than 2.5 % for peak height and 0.7 % for retention time in pre-concentration methods. This method Showed good reproducibility and reliability and it was thought the deviations of recovery value could be reduced by considering column capacity and making water sample homogeneous. Matrix Elimination could be done using the pre-concentration method if perchlorate were in complex matrix of sample.

• 한국식품위생안전성학회지
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• 제38권5호
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• pp.319-331
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• 2023

아미노글리코사이드계 항생제(Aminoglycosides, AGs)는 그람음성균과 양성균에 광범위하게 작용하는 동물용 의약품으로, 최근 배양육에 사용된다고 알려져 있어, 안전성 관리를 위한 분석법 마련이 반드시 필요하다. AGs는 고극성 화합물로 성분 간의 분리를 위해 이온쌍 시약(ion-pairing reagent, IPR)을 사용하고 있으나 IPR을 이동상에 첨가하는 기존 분석방법의 경우 용매가 흐르는 동안 질량분석기로 주입되는 IPR로 인해 기기적인 문제가 발생할 가능성이 높아, IPR를 바이알에 직접 첨가하는 분석방법을 검토하였다. 본 연구에서 10종 AGs 성분에 대한 분석방법을 확인하고 유효성을 검증하였다. 검출한계와 정량한계는 각각 0.0001-0.0038 mg/kg 와 0.004-0.011 mg/kg의 범위로 나타났으며, 0.01-0.5 mg/kg 범위 내의 직선성(R²)은 0.99 이상이었다. AGs의 시료 회수율을 확인하고자 소고기와 세포배양배지(cell culture medium) 매질에서 회수율과 상대표준편차로 나타낸 정밀도를 확인한 결과 각각 70.7-120.6% 및 0.2 to 24.7%로 나타났다. 기존의 이동상에 IP 첨가 방법과 비교하였을 때 유사한 수준으로 양호하였다. 검증된 AGs 분석법은 국내 유통되는 닭고기, 소고기, 돼지고기 15품목과 배양육 배지 첨가제 6품목에 적용해보았다. 그 결과 국내 유통되는 육류 15품목 모두 AGs 성분이 검출되지 않았으나, 세포배양배지에서 streptomycin은 695.85-1152.71 mg/kg, dehydrostreptomyci은 6.35-11.11 mg/kg로 검출되었다. 따라서 IRR을 바이알에 직접 첨가하는 LC-MS/MS 방식은 육류, 세포배양배지, 배지첨가제 중 AGs 분석 및 안전성 평가를 위한 기초자료로 활용될 것으로 기대된다.