• 방사선산업학회지
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• 제4권1호
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• pp.7-11
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• 2010

Clotrimazole [1-{(2-chlorophenyl)-diphenylmethyl}-1H-imidazole, CLT] has been reported to inhibit the proliferation of vascular endothelial and act as an in vitro anti-VEGF drug. It is also shown to inhibit angiogenesis in an animal model. The radioisotope labeled clotrimazole derivative can be utilized to monitor the physiologic processes of cancer. In this study, we synthesized [$^{18}F$]fluoride labeled clotrimazole derivatives as a new tumor imaging agent for PET. The references were prepared by a refluxing with clotrimazole and an excess of fluoroalkyltosylate in acetonitrile for 36 h and clotrimazole reacted with ditosylalkane to give precursors. [$^{18}F$]Fluoride labeled reaction was performed with precursor in Kryptofix[2.2.2]/$K_2CO_3$ for 10 min at $80^{\circ}C$. The radiolabeling mixture was passed through a silica Sep-Pak cartridge to remove $^{18}F^-$. The [$^{18}F$]F-clotrimazole derivatives were synthesized with a 20~25% yield. In the radiofluorination step, we used acetonitrile and DMSO as a solvent and observed a higher yield at the acetonitrile (25%) reaction compared with the DMSO reaction (5%).

• Bulletin of the Korean Chemical Society
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• 제27권9호
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• pp.1315-1322
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• 2006

The following study describes the gas chromatography-mass spectrometry (GC-MS) based screening and confirmation analysis of urinary androgenic steroids. Four commercially available solid-phase extraction (SPE) cartridges, Serdolit PAD-1, Sep-pak $C_{18}$, amino-propyl, and Oasis HLB, and three different extractive organic solvents, diethyl ether, methyl tert-butyl ether (MTBE), and n-pentane, were tested for sample preparation. Overall, Oasis HLB combined with MTBE extraction provided the highest recoveries in 39 of 46 total androgenic steroids examined and it showed a good extraction yield (>82.1%) for polar steroids, such as metabolites of fluoxymesterone, oxandrolone, and stanozolol, which gave a poor recovery in both n-pentane (9.2-64.3%) and diethyl ether (22.2-73.6%) extractions. All SPE sorbents tested showed potential, because they were efficient in extraction for most or selective steroids. When applied to positive urine samples based on the results obtained, the present method allowed selective and sensitive analysis for detection of urinary androgenic steroids. The experiments showed that the high-resolution MS method is clearly more efficient than the low-resolution MS technique for the detection of many urinary steroids. However, comprehensive sample clean-up procedures also might be needed especially in confirmation analysis to increase detectability.

• Asian-Australasian Journal of Animal Sciences
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• 제14권10호
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• pp.1465-1469
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• 2001

A sensitive high-performance liquid chromatographic method was developed to determine the content of cholesterol in milk and dairy products. To optimize separation of cholesterol, mobile phases including acetonitrile:2-propanol (8:1, v/v), acetonitrile:methanol (3:1, v/v), and acetonitrile:methanoI:2-propanol (7:3: I, v/v/v) were compared. Acetonitrile/methanol/2-propanol was superior to the other mobile phase systems for separating cholesterol. Liquid-liquid extraction (LLE) of cholesterol was simplified using a non-polar solvent, hexane, to remove interfering compounds, and had an excellent recovery $(100{\pm}1.0%)$ of cholesterol. A solid phase extraction (SPE) method using Sep-pak $C_{18}$ was developed and compared with LLE. The SPE method was rapid and highly reproducible. Both extraction methods were useful when used in combination with saponification of esterified cholesterol to facilitate total cholesterol determination. The detection limit of cholesterol was $0.01{\mu}g$. The newly developed HPLC method was rapid, simple, and accurate, and has advantages over the many methods commonly used.

• Archives of Pharmacal Research
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• 제26권5호
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• pp.416-420
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• 2003

The analytical method of antispasmodic agent tiropramide {$(\pm)\alpha$-(benzoylamino)-4-[2-(diethylamino)ethoxy]-N,N-dipropylbenzenepropanamide hydrochloride} was developed by gas chromatography/nitrogen-phosphorus detector (GC/NPD) in human plasma. Two kinds of tiropramide tablets were orally administered to volunteers by Latin square crossover design, and blood was withdrawn as designed schedule. The plasma of 1 mL was loaded on Sep-pak $C_{18}$ cartridge and eluted with methanol after washing with 30% methanol. The residue dissolved in 100 $\mu$L of methanol after evaporation was analyzed by GC/NPD. Precision (CV%) of intra-day was located within 2.6% and accuracy was less than 9.7%. Inter-day precision was below 8.7% and accuracy was relatively good as less than 14%. Plasma samples obtained from human volunteers were analyzed for the determination of tiropramide concentration by using this method. The method was sensitive, rapid and suitable enough to be applied for pharmacokinetic and bioequivalence studies of tiropramide in human volunteers.

• 한국물환경학회지
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• 제25권5호
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• pp.720-726
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• 2009

We investigated the most effective pre-treatment processes and LC/MS/MS condition for microcystins analysis. With a step-by-step pre-treatment, efficiencies of several established methods were compared. At the level of cell burst, sonication method was found to be the most efficient. As a mycrocystins first extraction solvent, 5% acetic acid showed the highest efficiency. An isolation and recovery rate of mycrocystins of ODS Sep-Pak $C_{18}$ cartridge was higher than HLB SPE cartridge. As a final elution solvent from cartridge, 100% MeOH had a better efficiency than others. Using a LC/MS/MS, effective analytical methods were established. C18 reverse column was used and gradient elution was performed with using acetonitrile, 0.1% formic acid as a mobile phase. We analysed to 0.8 mL/min flow rate fit to the $5{\mu}m$ particle size column and $55^{\circ}C$ housing temperature. The validity of established analytical method was evaluated that MDL as average $0.050{\pm}0.014{\mu}g/L$ and LOQ as average $0.160{\pm}0.045{\mu}g/L$ had a good sensitivity over 40 magnification rather than $2{\mu}g/L$ detection limit of HPLC.

• Archives of Pharmacal Research
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• 제28권4호
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• pp.463-468
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• 2005

The purpose of the present study was to develop a standard protocol for imidapril hydrochloride bioequivalence testing. For this reason, a specific LC-MS method was developed and validated for the determination of imidapril in human plasma. A solid-phase extraction cartridge, $Sep-pak^{R}$ C18, was used to extract imidapril and ramipril (an internal standard) from deproteinized plasma. The compounds were separated using a XTerra $MS^{R}$?C18 column ($3.5 {\mu}m, 2.1\times150 mm$) and $acetonitrile-0.1\%$ formic acid (67:33, v/v) adjusted to pH 2.4 by 2 mmol/L ammonium formic acid, as mobile phase at 0.3 mL/min. Imidapril was detected as m/z 406 at a retention time of ca. 2.3 min, and ramipril as m/z 417 at ca. 3.6 min. The described method showed acceptable specificity, linearity from 0.5 to 100 ng/mL, precision (expressed as a relative standard deviation of less than $15\%$), accuracy, and stability. The plasma concentration-versus-time curves of eight healthy male volunteers administered a single dose of imidapril (10 mg), gave an $AUC_{12hr}$ of imidapril of $121.48\pm35.81 ng mL^{-1} h$, and $C_{max} and T_{max}$ values of $32.59\pm9.76 ng/mL and 1.75\pm0.27 h$. The developed method should be useful for the determination of imidapril in plasma with sufficient sensitivity and specificity in bioequivalence study.

• 좋은식품
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• 통권169호
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• pp.104-115
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• 2002

한국산 검정콩의 종피색소를 1$\%$ HCL 용액으로 4$^{\circ}C$에서 24시간 추출하여0.45$\mu$mmembrane filter로 여과한 후 Sep-pak plus $C_{18}$ cartridge를 통과시켜 흡착된 색소성분을 메탄올로 용출시켜 30$^{\circ}C$에서 농축하여 실험을 실시하였다. 검정콩 세 가지 품종의 조색소액의 생리활성 효과를 살펴본 결과 고혈압에 관여하는 angiotensin converting enzyme 저해실험에서는 검정콩 1호, 일품검정콩 및 밀양 95호에서의 $IC_{50}$는 각각 0.22, 0.28, 0.38mg/mL로 나타나 검정콩 1호가 가장 우수하였다. 통풍에 관여하는 xanthine oxidase 저해실험에서의 $IC_{50}$이 각각 0.118, 0.165, 0.163mg/mL로 나타나 angiotensin converting enzyme 저해실험에서와 동일하게 검정콩 1호가 가장 높게 나타났다. 항염증효과를 살펴본 결과 $cPLA_2$를 50$\%$ 저해하는 $IC_{50}$값이 19.7, 10.7, 25.3$\mu$g/mL로 나타났으며, 암세포 증식 억제능을 실험한 결과 각각의 시료 중 밀양 95호가 0.5mg/mL의 농도에서 사람 유래의 결장암 세포주인 HT-29 및 사람과 마우스 유래의 간암 세포주인 HepG2와 Hepa에 대하여 각각 66.0$\%$, 58.2$\%$, 64.4$\%$의 억제능을 보여 시료 중 구성된 검정콩 1호보다는 여러 색소 성분이 공존하는 것이 더 유리한 결과를 나타내었으며, 여러 가지 가능성을 가지는 색소임을 알 수 있었다.

• 분석과학
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• 제11권5호
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• pp.321-331
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• 1998

기체크로마토그래피/질량분석법(GC/MS)을 이용하여 물시료 중에 미량으로 함유된 19종의 여러고리방향족탄화수소류에 대한 액체-액체 추출법, disk추출법 및 고체상 추출법을 이용한 시료 매트릭스로부터 분리, 추출하는 방법을 조사하였다. GC/MS의 오븐온도프로그램을 $80{\sim}310^{\circ}C$까지 단계적으로 변화시킨 결과 19종의 PAH류를 분리할 수 있었다. 액체-액체 추출법에 의한 물시료 중 PAH류의 회수율은 71.3~109.5% 범위로 나타났고, filtration에 의한 $C_{18}$ disk추출법의 회수율은 80.7~94.9% 범위로 높게 나타났다. 그러나 $C_{18}$ Sep-Pak을 사용한 고체상 추출법의 회수율은 51.8~77.9%범위이었다. 이상의 추출법에 대한 추출 회수율, 재현성 및 실험의 편리성 등 장단점을 비교한 결과, $C_{18}$ disk를 사용한 거르기법이 PAH류의 추출에 가장 적합한 방법임을 확인하였다. 각 추출법의 검출한계(S/N=5)는 액체-액체 추출법 및 고체상 추출법의 경우 0.25~6.25 ppb, disk추출법은 0.05~1.25 ppb 범위이었다.

• 한국식품영양과학회지
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• 제38권4호
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• pp.509-516
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• 2009

메주로부터 곰팡이 및 세균 등에 생육 저해활성을 나타내는 균주 B. polyfermenticus CJ6을 분리 동정하였다. 분리 균주 B. polyfermenticus CJ6는 2단 대수기를 나타내는 생육 곡선상 특이점을 나타내었으며 배양 30시간 이후부터 최대 활성을 나타내었고 사멸기 이후 활성이 다소 감소되었으나 120시간까지 활성을 유지하였다. B. polyfermenticus CJ6의 항진균 활성 물질은 $70^{\circ}C$ 이상에서 활성이 감소되었으나 $121^{\circ}C$에서 15분간 열처리 시 역가가 완전히 소실되지 않았다. pH 안정성 실험에서는 pH $3.0{\sim}9.0$ 구간에서 안정한 활성을 나타내었으며, 각종 효소에 대한 영향에서 항진균 활성물질은 proteinase K, protease, ${\alpha}$-chymotrypsin 등의 단백분해효소 처리로 역가를 상실하거나 일부 감소되어 단백질성 물질임을 추정하였다. 균주의 항진균 활성 물질을 $C_{18}$ Sep-Pak column으로 부분 정제한 후 Tricine-SDS-PAGE 및 direct detection 실험을 통하여 분자량이 약 1.4 kDa의 물질임을 확인하였다. B. polyfermenticus CJ6가 생산하는 항진균 활성 물질은 기존에 거의 보고되지 않은 B. polyfermenticus 유래의 단백질성 항진균 활성 물질로서 천연보존제 및 천연항균제재로 사용이 기대되며, 이를 위하여 항진균 활성 물질들의 정제 및 구조분석 등의 연구가 필요하다.

• Mycobiology
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• 제49권4호
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• pp.434-437
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• 2021

In our ongoing search for new secondary metabolites from fungi, a basidiomycete fungus Irpex consors was selected for mycochemical investigation, and three new zwitterionic alkaloids (1-3) and five known compounds (4-8) were isolated from the culture broth (16 l) of I. consors. The culture filtrate was fractionated by a series of column chromatography including Diaion HP-20, silica gel, and Sephadex LH-20, Sep-Pak C₁₈ cartridge, medium pressure liquid chromatography (MPLC), and high pressure liquid chromatography (HPLC) to yield eight compounds (1-8). The structures of the isolated compounds were elucidated by the interpretation of nuclear magnetic resonance (NMR) spectra and high-resolution mass spectrometry (HR-MS). Their antioxidant and antibacterial activities were examined. The zwitterionic structures of three new sesquiterpene alkaloids (1-3) were determined together with five known compounds identified as stereumamide E (4), stereumamide G (5), stereumamide H (6), stereumamide D (7), and sterostrein H (8). This is the first report of the zwitterionic alkaloids in the culture broth of I. consors. Three new zwitterionic alkaloids were named as consoramides A-C (1-3).