• 분석과학
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• 제11권5호
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• pp.386-393
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• 1998

란탄이온의 특성 발광선 세기가 TLC plate상에서 증폭되는 현상을 이용하여 $Dy^{3+}$ 이온에 대한 고감도의 미량분석법에 대하여 연구하였다. 수용액 상태에서의 $Dy^{3+}$ 이온의 발광선의 세기에 비하여 주어진 용액 시료를 TLC plate에 점적하면 이온의 방출선의 세기가 크게 증가하였다. 특히 점적된 이온에 o-Phenanthroline을 추가로 점적하면 방출선의 세기가 더욱 증가하는 증폭현상을 이용하여 $Dy^{3+}$ 이온의 검출한계를 용액 시료에 비하여 농도비로 약 10배 그리고 그 절대량으로는 $10^4$배 정도 개선하였으며 이때의 검정곡선은 검출한계 근처에서 $10^2$ order의 선형범위(dynamic range)와 상관계수가 0.99 이상인 직선성을 나타냈다. 한편 이러한 발광증폭의 이론적인 배경으로 착물내의 리간드와 란탄이온 사이의 energy-transfer mechanism을 설명하였다.

• 미생물학회지
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• 제35권1호
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• pp.41-46
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• 1999

수계에 분포하는 장바이러스를 검출하기 위해 민감도가 높고 검출시간이 빠른 PCR법을 이용하였다. 바이러스입자를 보다 순수하게 농축하기 위해 몇 가지 바이러스농축법을 비교조사하고 그것의 변형을 통하여 개선된 방법을 확립하였다. 비교한 농축방법중 흡탈착/Polyethyleneglycol(PEG) 침전법과 플록화/촉속원심분리법을 통해 10 PFU $ml^{-1}$ 까지 검출이 가능하여 다른 방법에 비해 효과적임이 판명되어Te. Sephadex resin을 이용한 부가적인 시료정제 과정을 통해 시료의 순도를 높일 수 있어검출한계를 10배정도 낮추었다. 서정된 검출법을 통해 한강수계에서 장바이러스의 분포를 조사한 결과 조사한 시료중 한강의 지천에서는 75%, 본류에서는 20%의 시료에서 바이러스가 검출되었다. 본 조사결과 흡탈착/PEG 침전법-PCR 검출기법이 수계의 바이러스 오염도를 간편하고 신속하게 검출하는데 매우 유용하였으며 국내 수계에도 바이러스 오염이 광범위함을 확인하였다.

• 한국환경보건학회지
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• 제45권3호
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• pp.258-266
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• 2019

Objectives: In this study, blood lead was analyzed using graphite furnace atomic absorption spectrometry (GF-AAs) and inductively coupled plasma mass spectrometry (ICP-MS). We tried to examine the difference and consistency of the analytical values and the applicability of the analytical method. Methods: We selected 57 people who agreed to participate in this study. After confirming the linearity of the calibration standard curves in GF-AAs and ICP-MS, the concentrations of lead in quality control material and samples were measured, and the degree of agreement was compared. Results: The detection limit of the ICP-MS was lower than that of GF-AAs. The coefficient of variation of reference materials was shown to be stable in the ICP-MS and GF-AAs. When the correspondence between the two equipments was verified by bias of the analysis values, a concordance was shown, and approximately 98% of the ideal reference lines were present within ${\pm}40%$ of the deflection. Conclusion: GF-AAs showed high sensitivity to single heavy metal analysis, but it took much time and showed higher detection limit than ICP-MS. Therefore, it would be considered necessary to switch to ICP-MS analysis method, considering that the level of lead exposure is gradually decreasing.

• 한방비만학회지
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• 제20권2호
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• pp.97-108
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• 2020

Objectives: Ephedra sinica and Wolbigachul-tang which contains Ephedra sinica are used to treat obesity in Korean medicine. The aim of this study was to analyze the quantities of ephedrine alkaloids by high-performance liquid chromatography. Methods: The analysis was performed using a YMC-Triat C18 column with operating at 25℃, and UV detection at 210 nm. The mobile phase used a gradient flow with 0.1% H3PO4 in water and acetonitrile. Specificity, linearity, precision, accuracy, limit of detection, and limit of quantification were measured for validation anaylsis. This method was applied to analyze the quantities of ephedrine alkaloids in Ephedra sinica and Wolbigachul-tang. Results: The concentration per Ephedra sinica (gram) of ephedrine and pseudoephedrine in Ephedra sinica decoction are 4.74±0.22 mg and 2.19±0.10 mg, respectively and in Wolbigachul-tang decoction are 6.39±0.34 mg and 2.97±0.21 mg, respectively. The retention time of ephedrine was 23.6 min and that of pseudoephedrine was 25.8 min, and norephedrine and methylephedrine were not detected. Conclusions: In conclusion, analyzed the concentration of ephedrine alkaloids in Ephedra sinica and Wolbigachul-tang by the developed validation method.

• Applied Biological Chemistry
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• 제41권8호
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• pp.595-599
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• 1998

An analytical method was developed to determine tricyclazole residues in rice grain, straw, and soil using high-performance liquid chromatography (HPLC) with ultraviolet absorption detection. Tricyclazole was extracted with methanol from moist rice grain, straw, and soil samples. n-Hexane washing was employed to remove nonpolar co-extractives during liquid-liquid partition. Tricyclazole was then extracted with dichloromethane from alkaline aqueous phase, while acidic interferences remained in the phase. Dichloromethane extract was further purified by silica gel column chromatography prior to HPLC determination. Reverse-phase HPLC using an octadecylsilyl column was successfully applied to separate and quantitate the tricyclazole residue in sample extracts monitored at ${\lambda}_{max}$ 225nm. Recoveries from fortified samples averaged $95.5{\pm}3.0%\;(n=6),\;87.5{\pm}20.%\;(n=6),\;and\;84.3{\pm}2.8%$ (n=12) for rice grain, straw, and soil, respectively. Detection limit of the method was 0.02 mg/kg for rice grain and soil samples while 0.05 mg/kg for rice straw samples. The proposed method was reproducible and sensitive enough to evaluate the safety of tricyclazole residues in rice grain, straw, and soil.

• 한국환경과학회지
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• 제4권3호
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• pp.97-97
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• 1995

PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

• 한국환경과학회지
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• 제4권3호
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• pp.249-258
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• 1995

PCBs have been measured using GC-ECD, GC-MS, GC-ELCD, HPLC, TLC, NMR and Immunoassay. The analysis of PCBs using GC-ECD include the peak pattern method as none derivatization and the Perchlorination method as derivatization. This study was conducted to establish the perchlorination method with Sbcls from PCBs to decachlorinated biphenyl(DCB). The aroclor 1242 of PCBs was chlorinated and then, converted into the DCB which showed a single peak in GC-ECD chromatogram. The detection limit of DCB was 2pg. The quantification detection concentration of PCBs extracted with soxhlet was 0.5ng/g in the soil. PCBs were not detected in the suburban soil, but 174ng/g in the soil of industrial complex. Mean PCBs concentration of Shinchun stream at Kumho river and Jinchun stream at Nakdong river was calculated average 낙ngjg in 각e sediment. PCBs concentration in the sediment of Kumho river near 2-7km from conjunction with Nakdong river was average 154ng/g. PCBs concentration in the sediment of Nakdong river near conjunction with Kumho river was average 159ng/g.

• Bulletin of the Korean Chemical Society
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• 제33권1호
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• pp.171-176
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• 2012

A novel chemiluminescence (CL) system was established for the determination of cytosine arabinoside (Ara-C) in pharmaceutical preparations. It was showed that a clear CL signal was observed when Eosin Y mixed with Fenton reagent. The CL intensity was decreased significantly when Ara-C was added to the reaction system and partially scavenged the hydroxyl radicals in the solution. The extent of decrease in the CL intensity had a good stoichiometrical relationship with the Ara-C concentration. Based on this, we developed a new method for the determination of Ara-C using a flow injection analysis (FIA) technique with CL detection. Under the optimal conditions, the linear range of Ara-C concentration was $6.0{\times}10^{-9}\sim1.0{\times}10^{-7}mol/L$ (R = 0.9982) with a detection limit of $7.6{\times}10^{-10}mol/L$ (S/N=3), the RSD was 5.6% for $6.0{\times}10^{-8}mol/L$ Ara-C (n = 11). The method was successfully applied to the determination of Ara-C in injection samples. The possible chemiluminescence reaction mechanism was discussed.

• 동아시아식생활학회지
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• 제16권5호
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• pp.585-591
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• 2006

We report a novel HPLC method for analyzing the capsaicinoids and nonivamide. The following conditions were used: a total column and column temperature of $3^{\circ}C$, a detection wavelength of 280 nm, an eluent containing acetonitrile : 0.5% formic acid(31:69, v/v). The experimental data was compared with standard nonivamide and capsaicin. The results showed that nonivamide was eluted in 96.7 minutes with a recovery ratio of 96.5% after adding known nonivamide. In addition, the detection limit for nonivamide was 18.6 ng. The capsaicinoids from Korean pepper were extracted (after blooming 60th) from 3 breeds cultivated in Korea, Buchon, Chungyang and Hanbando. and crisis it analyzed sympathizes the nonivamide in the result nonivamide from the Buchon and the Chungyang which are not detected from the Hanbando $0.16{\sim}0.24{\mu}g/g$ it detects with very small amount it contains it confirmed the each capsaicinoid with the HPLC and the LC-MS. These results are expected contribute to the quality control of various product processes, which includes product delivery inspection as well as examining the capsaicinoids present in the product for possible medicine manufacture and various foodstuff, and the nonivamide content, which may be a feed for various manufacturing processes involving chemical synthesis.

• Archives of Pharmacal Research
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• 제19권6호
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• pp.469-474
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• 1996

A rapid and sensitive method has been developed to detect hepatitis B virus DNA (HBV) by nested polymerase chain reaction (PCR) technique with primers specific for the surface and core regions in capillary thermal cycler within 80 min. The lower limit for detection by present PCR method is $10^{-5}$ pg of recombinant HBV DNA which is equivalent to that determined by one round of PCR amplification and Southern blot hybridization analysis. When boiled HBV positive serum was serially diluted 10-fold, HBV DNA was successfully determined in $1{\mu}l-10^{-3}$ of serum. HBV DNA was detected by present method in 69 clinical samples including HBsAg positives and negatives by enzyme-linked immunosorbent assay (ELISA). When serum samples were amplified by nested PCR using surface and core region primers, HBV DNAs were detected in 37 of 69 samples (53.6%) and 18 of 69 samples (26.1%), respectively. These results can inform the infectious state of HBsAg positive pateints. A simple and rapid nested PCR protocol by using boiled serum as DNA template has been described for the clinical utility to determine HBV DNA in human serum.