• 약학회지
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• 제55권1호
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• pp.64-68
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• 2011

In this study, a high performance liquid chromatography-diode array detector method was established, for simultaneous determination of three compounds, berberine, palmatine and geniposide in Hwangryunhaedok-tang, To develop and validate method, $C_{18}$ column (5 ${\mu}M$, 4.6 mm${\times}$250 mm) was used with gradient mobile phase, water containing 0.1% trifluoroacetic acid (TFA) and MeOH at the column temperature of $30^{\circ}C$. UV wavelength was set at 230 and 280 nm. Validation of the chromatography method was evaluated by linearity, precision and accuracy test. Calibration curve of standard components showed good linearity ($R^2$ > 0.9999). The limits of detection (LOD) and limits of quantification (LOQ) varied from 0.05 to 0.17 ${\mu}g/ml$ and 0.15 to 0.53 ${\mu}g/ml$, respectively. The relative standard deviations (RSDs) data of intra-day and inter-day test were in less than 2.99% and 1.90%, respectively. The results of the accuracy test were in the range of 98.36 to 102.52% with RSDs values 0.32 to 1.98%. The results of validation indicated that this method was a very accurate and sensitive assay.

• 한국약용작물학회지
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• 제24권6호
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• pp.451-457
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• 2016

Background: Leonurine is a the aerial part of Leonurus japonicus Houttuyn, which has been used as a traditional medicines and is registered in the Korean Pharmacopoeia. Methods and Results: In the present study we performed a heavy metals and thin layer chromatography and measured loss on drying, as well as the contents of total ash, acid-insoluble ash, ethanol soluble compounds, and leonurine, using 15 domestically collected L. japonicus samples. The methods were performed according to the 'crude drugs test of the general test, processes and apparatus', published by MFDS, Korea (2014). The purity test (heavy metals) indicated that levels of Pb and Hg were 0.35 - 3.64, and 0.001 ppm, respectively, whereas the levels of As and Cd were undetectable, and stachydrine was identified by thin layer chromatography ($R_f$ : 0.15). We found that 5.93 - 10.62% (average: $8.58{\pm}1.8%$) of the sample mass was lost during drying, and the contents of total ash, acid-insoluble ash, ethanol soluble compounds, and leonurine were 7.87 - 10.84% (average: $9.62{\pm}0.82%$), 0.99 - 1.76% (average: $1.38{\pm}0.24%$), 16.70 - 23.11% (average: $19.49{\pm}2.14%$) and 0.04 - 0.17% (average: $0.11{\pm}0.04%$) respectively. In addition, HPLC profiling detected leonurine (5.94 min), rutin (16.43 min) and myricetin (26.78 min). Conclusions: We hope that this the rusult of the present study will contribute to the standardization and quality control of Korean herbal medicines.

• 대한화학회지
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• 제8권2호
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• pp.85-87
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• 1964

Alloxan에 의한 Amino acids의 spot test에 있어서, alloxan수용액에 lactose를 가해주면, alloxan 자신의 착색을 막을 수 있다. lactose를 포함하는 alloxan수용액은 매우 안정하여서, 실온에서 수 개월 동안 두어도 착색되지 않으며, lactose의 존재로 말미암아, alloxan과 amino acids와의 색반응은 조금도 영향을 받지 않았다. 이시약에 의한 amino acids의 spot test법은 ninhydrin에 의한 spot test보다 예민하고, 또 alloxan 또는 dimethylalloxan을 발색약으로 사용하는 paper chromatography법에 비해, proline (1 ${\gamma}$), hydroxyprolin (5 ${\gamma}$)를 확인할 수 있다는 장점을 가지고 있다.

• 한국미생물·생명공학회지
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• 제27권3호
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• pp.215-222
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• 1999

Methylotrophic actinomycetes No. 155 produced an aminoglycoside antibiotics(AG)-resistant inhibitor. We have previously reported that the inhibitor shows strong inhibition to sisomicin-resistant strain. In order to understand the functions of inhibitor and sisomicin-resistance, characterizations and purification of inhibitor were investigated. Strain No. 155 was tentatively identified as Nocardiopsis sp. based on morphological and some physiological characteristics. In the antimicrobial activity test, the addition of inhibitor to sisomicin showed a reduction effect of MIC on the test strains such as Gram(+), Gram(-) bacteria and yeasts. The combination of the inhibitor and various antibiotics revealed synergistic against E. coli K-12 and B. subtilis PCI 219. The induced intracellular proteins from sisomicin-resistant strain exhibited the sisomicin inactivation by invitro test. And the induced intracellular proteins were inactivated by addition of the inhibitor. The inhibitor compound was purified by anion exchange chromatography(Dowex-1) and HPLC using Asahipak ES-502C column. The purified inhibitor compound was detected in a single peak(above 98.5% purity) through the HPLC analysis.

• 한국유체기계학회 논문집
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• 제17권6호
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• pp.69-73
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• 2014

To predict flow fields and chemical agent dispersion in urban area, wind tunnel experiments was performed. The agent was adopted MS (methyl salicylate) because the real chemical agent is unsafe. The exact concentration of methyl salicylate was generated by the commercial gas generator (STI-2500) and three different obstacle shapes were applied (i.e., rectangular, cylinder and pyramid). The concentration was measured with the qualified ion mobility sensor and gas chromatography. The data necessary for virtual test method of the real chemical agent were obtained.

• Tribology and Lubricants
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• 제18권5호
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• pp.319-323
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• 2002

Polyol esters were synthesized by condensation reaction of polyols (PE and DiPE) and linear acids such as valeric acid, caproic acid, heptylic acid and caprylic acid. The structures of polyol esters were confirmed by gas chromatography. Hot tube test was used test was used to measure thermal stability of polyol esters and its thermal properties depended on the structure of acid moiety contained in polyol esters.

• 약학회지
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• 제47권5호
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• pp.266-270
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• 2003

We evaluated four commercially available methamphetamine immunoassays for their relative cross-reactivities of amphetamine analogues in human urine: Abbott TDx, Vitalab Selectra and on-site test kits (Accusign MET, SD bioline MET). High cross-reactivities were shown at designer's drugs such as methylenedioxyamphetamine (MDA), methylenedioxymethamphetamine (MDMA) and methylenedioxyethylamphetamine (MDEA) in all of the tested immunoassays. Methoxyphenamine, fenfluramine and phentermine were positive in TDx and Selectra, but were not positive in on-site test kits. Pseudoephedrine, norpseudoephedrine, ephedrine, norephedrine, MDMA, MDA, fenfluramine and phentermine were detected by gas chromatography/mass spectrometry(GC/MS) in false positive urines. Since the overall specificity of any of the devices was not 100％, we found it is important to confirm any positive screening test result, so we developed simultaneous determination of amphetamine analogues in urines. After alkalinization of the urine samples with 6-N NaOH, the analytes were extracted using ethyl acetate, derivatized with pentafluoropropyl anhydride (PFPA) prior at GC/MS analysis.

• 한국식품과학회지
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• 제31권6호
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• pp.1654-1660
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• 1999

건칠(Rhus verniciflua STOKES)은 옻나무과(Anacardiaceae)에 속하는 옻나무(Rhus verniciflua STOKES)의 수액으로 한방에서는 구충, 복통, 통경, 변비의 목적으로 사용되어 왔다. 옻나무 75% 에탄올 추출물의 클로로포름 분획물을 phenolic 성분을 중심으로 분리하여 항산화 활성이 우수한 free phenolic acid 성분(RCF)을 가지고 silica gel column chromatography를 실시하여 RCF-11, RCF-13로 이름 붙이고, 분리된 획분은 Rancimat mathod에서 다른 획분보다 강한 항산화활성을 보였다. RCF-11은 다시 3개의 물질로, RCF-13은 1개의 물질로 분리되었다. 소분획으로 분리된 물질들은 전자공여능, Rancimat을 통한 유도기간의 측정과 liposome상에서의 TBA test를 통해 항산화 활성을 측정하였다. RCF-13-1은 74.1%로 가장 강한 활성을 나타내었고, RCF-11-2는 54.62%를 나타내어 같은 농도의 BHT(45.19%) 보다는 높은 전자공여능을 보였으며, BHA(73.47%), ${\delta}-tocopherol(75.48%)$과는 비슷한 전자공여능을 보였다. Rancimat test에서도 돈지를 기질로 하였을 때 RCF-11-1, RCF-11-2, RCF-11-3, RCF-13-1획분의 AI는 같은 농도에서 각각 1.17, 1.84, 2.68, 1.54로 RCF-11-3의 유도기간이 가장 길었다. Liposome상에 적용하였을 때도 RCF-11-3의 lipid peroxide inhi-bition(%)이 전자공여능과 유도기간의 결과와 같이 유지의 산패 지연 효과가 가장 우수하였다. 이 물질들은 mass 및 $^1H-NMR,\;^{13}C-NMR$통해 각각 gallic acid, butin, butein, sulfuretin으로 확인되었다.

• 한국식품영양과학회지
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• 제29권2호
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• pp.300-306
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• 2000

In the present studies, we assessed the stability of active components and toxicological safety of irradiated Angelica gigas Nakai(Danggui). In order to confirm the stability of active components in the ${\gamma}$-irradiated roots of Danggui, the quantitative analysis of decursin and decursinol angelate of ${\gamma}$-irradiated sample was carried out by high performance liquid chromatographic (HPLC) methods using reverse phase columns and normal phase columns. From the root of Danggui, decursin and decursinol angelate were isolated by a silica gel column chromatography(toluene : ether (1 : 1), Hexane : EtOAc(15 : 1)). And then the structures were confirmed in the 1H and 13C-NMR analysis. The HPLC chromatograms of decursin and decursinol angelate in ${\gamma}$-irradiated Danggui were similar with those of non-irradiated sample. In the examination of in vitro genotoxicity of the water extract from ${\gamma}$-irradiated Danggui using Salmonella reversion assay(Ames test) and micronucleus test in Chinese hamster ovary (CHO) cells, mutagenicity was not exhibited in the two assays with or without metabolic activation. These resutls suggest that active components in the ${\gamma}$-irradiated Danggui should be stable and that the safety of ${\gamma}$-irradiated Danggui could be revealed in further test in vivo.

• 한국식품과학회지
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• 제20권6호
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• pp.856-861
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• 1988

본 실험은 Staphylococcus aureus의 한 균주로부터 A와 C, 두 종류의 toxin이 동시에 생성될 때 이들의 동시분리를 위하여 각종 분리방법을 연구하였다. 혼합된 toxin A와 C는 CM-column chromatography를 이용하여 pH-gradient법으로 용출했을 때 2개의 분획이 나타났으나 서로 완전히 분리되지 않아 다량의 서로 다른 toxin이 함유되어 있었고 Sephadex G-75, Sephacryl S-300, 그리고 ultro gel을 사용한 gel filtration에서는 하나의 분획을 나타내 상호분리가 불가능 하였으며 정제도와 분리도에서 가장 뛰어난 gel column을 이용한 FPLC도 toxin A와 C를 상호분리할 수 없었다. 그러나 CM-column을 이용한 FPLC에서는 enterotoxin A는 pH 6.8에서 그리고 enterotoxin C는 pH 8.6에서 각각 분리되었으며, immunodiffusion test 결과 enterotoxin A의 분획에서는 toxin C가 전혀 검출되지 않았고 enterotoxin C의 분획에서도 toxin A가 검출되지 않았다. 용출방법에 있어서는 CM-column을 이용한 FPLC에서 pH-stepwise법이나 pH-gradient법으로 enterotoxin A와 C type을 쉽게 동시에 분리할 수 있었다.