• Journal of the Korean Chemical Society
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• v.54 no.5
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• pp.523-532
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• 2010

The proposed method is simple, sensitive and specific Liquid chromatography-tandem mass spectrometry (LCESI-MS/MS) method for the quantification of Entacapone (EA) in human plasma using Entacapone-d10 (EAD10) as an internal standard (IS). Chromatographic separation was performed on Zorbax SB-C18, $2.1{\times}50\;mm$, $5\;{\mu}m$ column, mobile phase composed of 10 mM Ammonium formate (pH 3.0): Acetonitrile (60:40 v/v), with a flow-rate of 0.7 mL/min, followed by Liquid-liquid extraction. EA and EAD10 were detected with proton adducts at m/z $306.1{\rightarrow}233.1$ and $316.3{\rightarrow}233.0$ in multiple reaction monitoring (MRM) positive mode respectively. The method was validated over a linear concentration range of 1.00 - 2000.00 ng/mL with correlation coefficient ($r^2$) $\geq$ 0.9993. Intra and inter-day Precision within 3.60 to 7.30 and 4.20 to 5.50% and Accuracy within 97.30 to 104.20 and 98.30 to 105.80% proved for EA. This method is successfully applied in the bioequivalence study of healthy Indian human volunteers.

• Journal of the Korean Chemical Society
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• v.34 no.1
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• pp.44-50
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• 1990

The liquid chromatographic retention behavior of structural isomers of phenols was investigated by a change of the mobile phase properties. The retention behavior of structural isomer of phenols in reversed phase liquid chromatography was affected by eluent electrolyte added. It can be seen that this behavior is illustrated by a mechanism of Langmuir isotherm and ion exchange between phenolate and the reversed phase coated with ions. The retention behavior was represented as two different areas according to the concentration of the electrolytes. These areas can be explained as counter ion and co-ion effect, respectively. The maximum retention values were dependent not upon the kinds of organic modifier but upon the kinds of electrolyte.

• Journal of the Health Care and Life Science
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• v.9 no.1
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• pp.141-146
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• 2021

Determination of capsaicin, dihydrocapsaicin and nonivamide in pungent liquids of self-defense spray were studied. The nonivamide having almost same spicy taste with capsaicin have been containing a few amounts in natural products, it had called as synthetic capsaicin or PAVA, have used to flavorings for foodstuffs and incapacitating agents of riot controls. Nowadays, it has been occasionally found that the quality controls of a self-defense sprays were not properly due to flood of illegal self-defense sprays. Thus, the simple analytical method with gas chromatography is developed, it is identified whether the products which have contained synthetic capsaicin were marked like natural materials as well as the pungent ingredients in it obeyed with permissible concentration to human or not was investigated. Finally, the pungent components and amounts in some kinds of self-defense spray were investigated.

• Applied Biological Chemistry
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• v.47 no.1
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• pp.22-26
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• 2004

The ligninolytic basidiomycete, Pleurotus ostreatus K-2946, was produced a manganese peroxidase (MnP) activity when grown in liquid culture with glucose-yeast-peptone (G-Y-P) medium. However, lignin peroxidase (LiP) was not detected in this culture medium. The purification progress of MnP was purified that included chromatography on Sepharose CL-6B, Superdex 75 prep grade and Mono-Q. MnP purified by column chromatography, was 36400 dalton and a pI of 3.95. The optimal pH and temperature of the purified MnP activity were 5.0 and $55^{\circ}C$. The characteristics of MnP produced was quite similar to those of MnP 3 isoenzyme produced by other strains of P. ostreatus.

• Analytical Science and Technology
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• v.18 no.1
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• pp.13-22
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• 2005

The elution patterns of seventeen 2,3,7,8-substituted PCDDs/Fs and 12 dioxin-like PCBs were studied by both manual open columns and automatic parallel LC columns in cleanup procedure. PCDDs/Fs and non-ortho-PCBs from other mono-ortho-PCBs were separated on automatic LC column, whereas they were not separated on an open manual column. The elution study on two cleanup methods was carried out using the PAR solution of unlabeled congeners and checked the recovery of each congener. Total recoveries of cleanup fractionation were ranged between 61.9 ~ 96.0% for PCDDs/Fs and 70.4 ~ 79.0% for PCBs by manual open columns and 71.8 ~ 104.5% for PCDDs/Fs and 61.3-120.3% for PCBs by automatic parallel LC columns, respectively. Unfortunately, #169-HxCB and 1,2,3,7,8-PeCDD were not separated on DB-5MS capillary column. The ions of 1,2,3,7,8-PeCDD were selected at M/M+2 instead of M+2/M+4 suggested by EPA method 1613. It is possible to discriminate 1,2,3,7,8-PeCDD and PCB #169 in HRGC/HRMS analysis.

• Analytical Science and Technology
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• v.7 no.3
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• pp.379-386
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• 1994

The elution behaviors in reversed-phase liquid chromatography were investigated thermodynamically for 2-hydroxy-arylazopyrazolone chelates with Ni(II), Cu(II), Co(III), Cr(III) on Novapak $C_{18}$ column. There was a good linear dependence of the capacity factor(k') on the variations of column temperature in van't Hoff plot. From this result, it was confirmed that the retention mechanism of these chelates in the reversed phase liquid chromatography system was invariant under the condition of various temperatures. For the most cases of the chelates studied, the dependence of capacity factor(1n k') on enthalpy$(-{\Delta}H)^{\circ}$, calculated by van't Hoff plot showed a good linearity(r=0.980~0.999) except [Pm(2-OH_(5-Cl)PaPz](r=0.787) and also the compensation temperatures(${\beta}$) showed constant values. The range of compensation temperature values calculated from the slope of $-{\Delta}H^{\circ}$ vs 1n k' plots was 374.3~806.9K. It was suggested that the retention of metal-2-hydroxy-arylazopyrazolone chelates in the reversed phase liquid chromatography system was largely affected by the hydrophobic effect.

• Journal of the Korean Chemical Society
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• v.37 no.4
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• pp.453-461
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• 1993

Detection method was developed using a simply designed photochemical reactor made of teflon coil and low pressure mercury lamp. This method of UV photolysis of analytes followed by UV, fluorescence and electrochemical detection was found to be useful for four thiocarbamates. Analytes eluting from the column are irradiated with a high flux of 254 nm UV light, so that they change to either fluorescent active forms or highly electrochemically sensitive products. Appling this technique to the UV detection, thiocarbamates were converted into long wavelength absorbing products upon UV irradiation. In fluorescence detector four thiocarbamates are not detected at nonirradiated condition but fluorescence signals of MPTC, CPTC photolysates are appeared after irradiation with UV light. The electrochemical detection for the determination of thiocarbamates was enhanced up to 5∼20 fold signal after UV irradiation, compared to that of the nonirradiated. The detection limit of thiocarbamates on electrochemical detector was 13.3∼0.02 ng under pH 7.0, ionic strength $0.5{\times}10^{-2}$ M, phosphate buffer solution. Adducts produced by reaction of photolysates and OPA-MERC in the reaction coil were monitored at 425 nm with fluorescence detector, and one of the photolysates was primary amine.

• Journal of the Korean Chemical Society
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• v.49 no.4
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• pp.349-354
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• 2005

• Journal of the Korean Chemical Society
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• v.63 no.5
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• pp.387-391
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• 2019

• Proceedings of the Korean Society of Applied Pharmacology
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• 1994.04a
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• pp.179-179
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• 1994

새로운 항생물질을 개발하기 위하여 토양으로부터 분리한 균주를 액체 및 고체배지에서 배양하여 여러 검정균에 대하여 종이디스크법으로 항균효력을 조사하였다. 그 결과 (+), G(-), fungi 등에 강한 항균 효력을 보인 토양균 SNUS 8810-43과 Mycobacterium, fungi에 항균력을 보인 토양균 SNUS 8810-129를 선택하여 각각의 배양액에서 항생물질을 분리하고, 분리한 항생물질의 구조를 규명하고자 하였다. 토양균 SNUS 8810-43의 배양액으로부터 항생물질을 분리하기 위하여 양이온 교환 수지 관 크로마토그래피와 셀룰로오스 관 크로마토그래피를 수행하여 시료 JJH-II-46-43을 얻었다. 시료 JJH-II-46-43의 IR, $^1$H-NMR, $^{13}$C-NMR, $^1$H-$^1$H COSY, $^1$H-$^{13}$C COSY, FAB-MS 스펙트럼을 얻어 분리한 항생물질의 구조를 분석하여 이 항생물질의 구조가 N-methylstreptothricin과 동일하다는 것을 확인하였다. Mycobacterium smegmatis에 강한 활성을 나타내는 물질을 토양균 SNUS 8810-129로 부터 분리하였다. 토양균 SNUS 8810-129를 배양한 V-8 아가판을 메탄올로 추출하여 이를 실리카겔 관 크로마토그래피와 preparative TLC로 시료 LCH-IV-17B, LCH-III-387을 얻었다. 시료LCH-IV-l7B, LCH-III-387의 $^1$H-NMR, $^{13}$C-NMR, FAB-MS, CI-MS, IR등의 스펙트럼을 얻어 분리한 항생물질의 구조를 분석하여 이 항생물질이 glycolipid계 항생물질이라는 것을 알았다. $^{13}$C-NMR 상의 자료와 화학적인 방법으로 구성당을 조사한 결과 이 항생물질을 이루고있는 당은 rhamnose 임을 알았다. 또 이 항생물질을 구성하는 지방산은 화학적인 방법과 MS 스펙트럼, $^{13}$C-NMR 스펙트럼으로부터 hydroxydecanoic acid인 것으로 확인되었다. 항생물질 LCH-III-387와 항생물질 LCH-IV-l7B는 각각 rhamnose를 1, 2개 포함하고 있는 것으로 확인되었다. 그리고 동일한 탄소수의 지방산을 가지고 있는 것으로 생각되었다. 이들 항생물질을 이루는 구성당과 지방산간의 정확한 연결및 구조, 생리활성에 관한 연구는 계속 수행중에 있다.