• Bulletin of the Korean Chemical Society
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• 제29권6호
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• pp.1185-1189
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• 2008

Two HPLC methods such as cefadroxil and cefalexin methods were compared in their performance for the quantitative analysis of the content and purity of $\beta$ -lactamic antibiotic, cefradine, for six bulk drug samples. Between the two methods, the cefadroxil method prescribed by the European Pharmacopoeia (EP) for the determination of impurities in cefradoxil was superior to the cefalexin method prescribed by the EP and by the United States Pharmacopeia (USP) for the determination of cefalexin impurity in cefradine in terms of the greater stability of the chromatogram baselines and the higher precision, i.e., the lower % relative standard deviation (RSD). Based on the comparison of the two HPLC methods, the cefadroxil method was recommended to replace the TLC method, which has been prescribed by the EP as the official method for determination of extraneous impurities in cefradine.

• 상하수도학회지
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• 제18권5호
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• pp.628-637
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• 2004

In many drinking water treatment plants, chlorination process is one of the main techniques used for the disinfection of water. This disinfecting treatment leads to the formation of disinfection by-products (DBPs) such as haloacetonitriles (HANs), trihalomethanes (THMs), haloacetic acids (HAAs). In this study, headspace-solid phase microextraction (HS- SPME) technique was applied for the analysis of HANs in drinking water. The effects of experimental parameters such as selection of SPME fiber, the addition of salts, magnetic stirring, extraction temperature, extraction time and desorption time on the analysis were investigated. Analytical parameters such as linearity, repeatability and detection limits were also evaluated. The $50/30{\mu}m$-divinylbenzene/carboxen/polydimethylsiloxane fiber, extraction time of 30 minutes, extraction temperature of $20^{\circ}C$ and desorption time of 1 minute at $260^{\circ}C$ were the optimal experimental conditions for the analysis of HANs. The correlation coefficients ($r^2$) for HANs was 0.9979~0.9991, respectively. The relative standard deviations (%RSD) for HANs was 2.3~7.6%, respectively. Detection limits (LDs) for HANs was $0.01{\sim}0.5{\mu}g/L$, respectively.

• Korean Chemical Engineering Research
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• 제54권5호
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• pp.636-647
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• 2016

Magnetite nanoparticles ($Fe_3O_4$ NPs) were synthesized by co-precipitating method under optimized condition. The $Fe_3O_4$ NPs coated with sodium dodecyl sulfate-thenoyltrifluoroacetone ($Fe_3O_4$ NPs-SDS-TTFA) were then exerted as the magnetic solid phase extraction (MSPE) adsorbent for the extraction process prior to introducing to a flame atomic adsorption spectrometry (FAAS). The synthesized $Fe_3O_4$ NPs-SDS-TTFA were applied for the extraction of Pb(II) ions from different water samples. The characterization studies of nanoparticles were performed via scanning electron microscopy-energy dispersive micro-analysis (SEM-EDAX), X-ray diffraction (XRD) and vibrating sample magnetometer (VSM) techniques. The substantial parameters affecting the extraction efficiency were surveyed and optimized. A dynamic linear range (DLR) of $10-400{\mu}g\;L^{-1}$ was obtained and the limit of detection (LOD, n=7) and relative standard deviation (RSD%, n= 6, $C=20{\mu}g\;L^{-1}$) were found to be $2.3{\mu}g\;L^{-1}$ and 1.9%, respectively. According to the results, the proposed method successfully applied for the extraction of Pb(II) ions from different environmental water samples and satisfactory results achieved.

• Bulletin of the Korean Chemical Society
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• 제27권10호
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• pp.1557-1561
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• 2006

The use of chemically modified silica-salen$(NEt_2)_2$ was studied for the separation and concentration of the metal ions from an aqueous solution by a solid phase extraction. After the salen(NEt2)2 was synthesized, it was chemically bonded to silica gel by a diazonium coupling reaction. The adsorption capacities and binding constants were obtained with respect to Cu(II), Mn(II), Pb(II) and Zn(II) by a graphical method. Some experimental conditions were optimized for the determination of the trace elements. After the silica-salen(NEt2)2 was pulverized in a sample solution of which the pH was adjusted, the solution was stirred to pre-concentrate the metal ions. The metal ions adsorbed were desorbed with nitric acid solution. And the concentrated analytes were determined by a flame AAS. The method proposed here was so rarely influenced by a sample matrix that the procedure was applied to 3 types of water samples. The reproducible results of less than 10% RSD were obtained at the concentration level of ca. 100 ng/mL and the recoveries of 95-109% were obtained in the spiked samples in which given amounts of analytes were added.

• 분석과학
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• 제11권2호
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• pp.96-104
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• 1998

수 많은 광검출기들이 직선으로 집적된 광다이오드 어레이를 이용한 모세관 전기영동장치용 다채널 검출기를 개발하였다. 본 연구에서 사용된 광다이오드 어레이는 1024개의 광검출소자를 가지고 있으며 275~675 nm 파장범위에서 시료의 흡수분광스펙트럼을 검출할 수 있다. 이 장치는 30 ms내에 전 파장영역의 스펙트럼을 얻을 수 있으며, PC에 의하여 시료분석에 필요한 여러 가지 조건들을 제어할 수 있도록 설계하였다. 개발된 검출기의 성능을 L-ascorbic acid와 alizarin yellow GG를 사용하여 시험하였다. 본 연구에서 개발한 모세관 전기영동장치용 다채널 검출기의 재현성 실험결과 상대 표준편차는 5.6%이었다.

• 한국축산식품학회지
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• 제29권4호
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• pp.482-486
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• 2009

The aim of this study was to optimize a simple, fast, and economical analysis procedure for the determination of 16 different pesticides in raw milk via GC/MSD. Analyses were performed via gas chromatography with electron impact mass spectrometric detection in the selected ion monitoring mode (GC/MSD-SIM) using Pentachloronitrobenzene as the internal standard. The modified sample preparation methodology was based on the Pesticide Analytical Manual (PAM) of the FDA concerning fat extraction, ACN-ether partitioning, and clean-up of the Sep-Pak florisil cartridge. The modified methodology for the determination of the 16 pesticides was validated. The range of LOQs of the 16 pesticides was likely three times lower than their Maximum Residence Levels (MRLs). The recoveries of most of the pesticides were acceptable at the fortification levels of 0.5 and 1.0 ${\mu}g/mL$ and their RSD (%) level was less than 20%. None of the 16 pesticides were detected in the selected raw milk samples.

• Toxicological Research
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• 제29권3호
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• pp.211-215
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• 2013

The trace toxic metal copper was assayed using mercury immobilized on a carbon nanotube electrode (MCW), with a graphite counter and a reference electrode. In this study, a macro-scale convection motor was interfaced with a MCW three-electrode system, in which a handmade MCW was optimized using cyclic- and square-wave stripping voltammetry. An analytical electrolyte for tap water was used instead of an expensive acid or base ionic solution. Under these conditions, optimum parameters were 0.09 V amplitude, 40 Hz frequency, 0.01 V incremental potential, and a 60-s accumulation time. A diagnostic working curve was obtained from 50.0 to 350 ${\mu}g/L$. At a constant Cu(II) concentration of 10.0 ${\mu}g/L$, the statistical relative standard deviation was 1.78% (RSD, n = 15), the analytical accumulation time was only 60 s, and the analytical detection limit approached 4.6 ${\mu}g/L$ (signal/noise = 3). The results were applied to non-treated drinking water. The content of the analyzed copper using 9.0 and 4.0 ${\mu}g/L$ standards were 8.68 ${\mu}g/L$ and 3.96 ${\mu}g/L$; statistical values $R^2$ = 0.9987 and $R^2$ = 0.9534, respectively. This method is applicable to biological diagnostics or food surveys.

• 한국연초학회지
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• 제33권1호
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• pp.21-27
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• 2011

Amadori compounds(1-deoxy-1-amino-2-ketoses) are important precursors of color, flavor and aroma produced in foods. Amadori compounds occur naturally in tobacco. The contribution of amadori compounds to smoke quality has been (of) interest because of their roles of the Maillard reaction in the leaf chemistry. The amounts of these compound in tobacco are affected by the processes of aging, drying and storage conditions. In this study, eight compounds were chemically synthesized because amadori compounds (have not been sold commercially these days.) were not available for obtaining commercially. The aim of this study was to develop the analytical method of amadori compounds in tobacco leaf by the liquid chromatography mass spectrometry using triple quadrupole analyzer(LC-MS/MS). This method was simple, rapid, selective and sensitive, and eight amadori compounds were simultaneously and quantitatively analyzed within 20 minutes. This method showed excellent accuracy and precision. Recovery rates of amadori compounds ranged from 86% to 102%, with relative standard deviation(RSD) ranged from 2.6% to 5.9%. This method was applied to analysis of amadori compounds contents of tobacco leaves in different varieties. Furthermore, it was expected that the method could be extended to the analysis of other amadori compounds.

• Journal of Pharmaceutical Investigation
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• 제41권1호
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• pp.25-30
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• 2011

Recently, Korean Food and Drug Administration (KFDA) has focused on developing quality control guidelines for all commercial products in Korea to enforce regulations, improve the quality control, and protect consumers by developing prevalently used and efficient analytical tools to determine and quantify target compounds. Because the Korean Pharmacopeia (KP) presents microbiological assays for biotin, which is laborious and time-consuming, this study is focused on applying HPLC-UV to detect and quantify biotin in complex drugs and dietary supplements like multi-vitamin. Biotin in complex drugs was extracted from methanol and analyzed using mobile phase with 10 mM potassium phosphate (monobasic, pH=3.0) in distilled water and acetonitrile. Gradient condition was used to successfully detect and quantify biotin within 20 minutes. Validation result for linearity was significant that average $r^2$ was 0.999 (n=3) and its relative standard deviation (RSD) was 0.0578% which was less than 2%. Using this method, quantification of biotin in complex drugs was completed successfully and recovery tests were finished that recovery percentage greater than 95% with relative standard deviation less than 2%.

• 한국대기환경학회지
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• 제10권1호
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• pp.24-31
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• 1994

Hourly variation of gaseous nitrous acid( HNO$_2$) concentration in Seoul air was monitored from Jan. 11 to SeP. 12, Nitrous acid concentration was determined by DS/IC over nine months of observation, HNO$_2$ range from 0.04 ppb to 5.5 ppb. Gor-tex tube as gaseous HNO$_2$generator in this study is thought to be more convenient and reproducible device than previous generator. As a result of NaOH instead of Na$_2$ CO$_3$/NaHCO$_3$ solution as the IC eluent, we could obtain more stable baseline. The concentration of the NaOH eluent was 15 mM . The limit of detection(3$\sigma$) of the liquid- Phase and gas phase nitrous acid of this method are 1.1ng/$m\ell$ , 0.04 n $\ell$ / $\ell$, respectively. The precisions evaluated by 10 replicate analysis of standard solution and standard gas generated are $\pm$1.59, $\pm$2. 89% RSD, respectively. Due to the lack of standard material for air, direct assessment of the accuracy was not possible. This study was applied to the analysis of Seoul ambient air and their results are reported herein.