• Bulletin of the Korean Chemical Society
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• 제30권4호
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• pp.945-947
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• 2009

• Biotechnology and Bioprocess Engineering:BBE
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• 제9권1호
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• pp.47-51
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• 2004

Ceramide III was prepared by the cultivation of Saccharomyces cerevisiae. Ceramide III was partitioned from the cell extracts by solvent extraction and analyzed by Normal Phase High Performance Liquid Chromatography (NP-HPLC) using Evaporative Light Scattering Detector (ELSD). We experimentally determined the mobile phase composition to separate ceramide III with NP-HPLC. Three binary mobile phases of n-hexane/ethanol, n-hexane/lsoprophyl Alcohol(IPA) and n-hexane/n-butanol and one ternary mobile phase of n-hexane/IPA/methanol were demonstrated. For the binary mobile phase of n-hexane/ethanol, the first mobile phase composition, 95/5(v/v), was step-increased to 72/23(v/v) at 3 min. In the binary mobile phase, the retention time of ceramide III was 7.87min, while it was 4.11 min respectively in the ternary system, where the mobile phase composition of n-hexane/IPA/methanol, 85/7/8(v/v/v), was step-increased to 75/10/15(v/v/v) at 3 min. However, in the ternary mobile phase, the more peak area of ceramide III was observed.

• KSBB Journal
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• 제15권5호
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• pp.537-540
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• 2000

일반적으로 paclitaxel과 유사한 구조를 가진 복잡한 유도체의 분리나 최종 제품에서의 엄격한 규정 등으로 인하여 한 단계의 HPLC system으로 정 제하는 것은 상당히 어렵다. 이러한 이유로 두 단계 HPLC system으로 식물세포 배양액으로 부터 paclitaxel의 대량 정제를 수행하였다. 즉, 첫번째 단계에 서 reverse-phase HPLC column, 두번째 단계에서 normal­p phase HPLC column을 사용하여 최종 제품을 얻었다. 또한 최종 정 제 된 paclitaxel 내 에 포함되어 있는 불순물 profile 확 언, 함량 분석, 그리고 이들 물질들에 대한 분리, 정제 및 동 정을 실시하였다 이들 불순물들 중에서 0.1% 이상되는 것은 모두 6종 (side chain derivative, baccatin III, 10-deacetyltaxol, cephalomannine, taxane derivative, 7-epitaxol)이며 NMR과 MS를 사용하여 화학구조를 분석한 결과 이미 알려진 pacli­t taxel 유도체 또는 전구체와 동일한 물칠로 밝혀 졌다. 본 연구 결과는 결국 paclitaxel 생산을 위한 품질관리 (quality con­t tr이)와 허가를 위한 자료로 유용하게 사용되어 진다.

• 분석과학
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• 제10권6호
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• pp.445-452
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• 1997

뇨 중에 Putrescine, Spermidine 및 Spermine benzoyl chloride를 유도체화제로 처리한 다음 HPLC법으로 정량하였다. ${\mu}$-Bondapak $C_{18}$ 컬럼과 methanol/$H_2O$(50/50v/v)를 사용하여 정상인 및 자궁암 환자의 뇨 중에서 Putrescine, Spermidine 및 Spermine을 역상법으로 분석한 결과 암환자의 경우 정상인에 비해 이들 polyamine이 현저한 증가를 보였다.

• 약학회지
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• 제41권4호
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• pp.414-420
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• 1997

A rapid and sensitive high performance liquid chromatographic method with UV detection for the analysis of polyamines(putrescine, spermidine, spermine) has been developed. The benzoyl chloride derivatives of putrescine, spermidine and spermine are separated on a mc-Bondapak C18 reverse-phase column with 50% methanol as the mobile phase. This method was applied to the analysis of polyamines in the serum of normal human and uterine cancer patients. The results show that the mean level of polyamines in cancer patients serum is much higher than that in normal human serum.

• 약학회지
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• 제50권1호
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• pp.21-25
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• 2006

Reiterated normal-phase column chromatography lead to the isolation and purification of six known compounds but for the first time from the whole plant of Sasa borealis (Hack.) Makino (Gramineae): tricin 4'-O-(erythro-${\beta}$-guaia-cylglyceryl) ether (1), tricin 4'-O-(threo-${\beta}$-guaiacylglyceryl) ether (2), tricin 4'-O-[erythro-${\beta}$-guaiacyl-(9'-O-acetyl)-glyceryl] ether (3), tricin 4'-O-[threo-${\beta}$-guaiacyl-(9'-O-acetyl)-glyceryl] ether (4), (-)-pinoresinol (5), and vanillin (6). The structures of the compounds (1-6) were established based on interpretation of high resolution NMR (COSY, HSQC, HMBC, and NOESY) spectral data. In particular, compounds 1 and 3 were diastereomers of compounds 2 and 4, respectively. These two sets of diastereomers were able to be simultaneously identified and quantified by a gradient reversed-phase HPLC method with UV photodiode array, This sensitive HPLC method is noteworthy as a simultaneous separation and identification method to test the extract of the family Gramineae which contains these compounds.

• 한국작물학회지
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• 제53권spc호
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• pp.115-120
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• 2008

비타민 vitamin E 구성 성분으로 항산화, 항암, 고지혈증 개선 등 다양한 생리활성을 나타내는 tocotrienol이 국내산 차조기에서 보고된 바, 존재 여부 확인을 위하여 국내수집 6종, 일본수집 8종 등 총 14종의 차조기 유전자원과 들깨 종실을 대상으로 HPLC 및 GC, GC/MS 비교 분석을 수행 하였으며 그 결과는 다음과 같다. 1. 순상의 HPLC 이용시 차조기에서 4종의 tocopherol 및 ${\beta}-tocotrienol$, ${\gamma}-tocotrienol$과 매우 유사한 머무름 시간의 발견되었다. 2. 그러나 동일 시료를 GC로 재분석한 결과 13개 차조기 유전자원에서 모두 4종의 tocotrienol과 일치하는 물질은 발견되지 않았다. 3. GC 이용시 ${\delta}-tocotrienol$ 및 ${\gamma}-tocotrienol$과 유사한 머무름 시간의 peak가 검출되었으나 GC/MS를 이용하여 확인한 결과 tocotrienol이 아닌 것으로 확인되었다. 4. 이상의 HPLC 및 GC 비교분석결과에 기초할 때, 차조기에는 tocotrienol류의 vitamin E는 존재하지 않는 것으로 추정되었으며 GC를 이용한 vitamin E isomer 분석이 HPLC 이용시 발생가능한 유사 머무름시간대 물질을 tocotrienol로 판단하는 오류 방지에 효과적임을 알 수 있었다.

• Applied Biological Chemistry
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• 제33권4호
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• pp.307-314
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• 1990

Brassinosteroid는 특이한 생리작용을 갖는 식물의 신 생장조절물질로 주목을 받고 있으나, 아직 우리나라의 가장 중요한 작물인 벼의 brassinosteroid에 대해 연구된 바 없어, 일반계 품종의 벼를 대상으로 brassinosteroid활성물질의 검색을 시도하였다. 동진벼와 영산벼를 최고분얼기까지 재배하여 지상부를 수확하고, 유기용매로 추출하여 얻어진 추출물에서 rice lamina inclination test에 의한 생물검정법으로 활성이 인정되어, 활성본체의 구명과 정제의 목적으로 각각의 활성획분을 silica gel 흡착 chromatography, Sephadex LH-20 chromatography, charcoal 흡착 chromatography, preparative TLC, Bondesil chromatography 그리고 normal, reverse phase의 HPLC 등적 방법으로 분획하여 검정한 결과 2품종 모두 brassinosteroid활성물질을 생산하고 있으며, 또 2품종간의 endogenous brassinosteroid의 유사성이 인정되었다.

• Journal of Pharmaceutical Investigation
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• 제39권3호
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• pp.177-183
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• 2009

A rapid and sensitive reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of piroxicam in the rabbit plasma. After a treatment of plasma sample by liquid-liquid extraction, the drug was analyzed on an HPLC system with ultraviolet detection at 330 nm. HPLC was carried out using reversed-phase isocratic elution with a C18 column, a mobile phase of a mixture of acetonitril, doubly deionized water and acetic acid 43.74:56.00:0.26 v/v%) at a flow rate of 1.1 mL/min. The chromatograms showed good resolution and sensitivity and no interference of plasma. The calibration curve for the drug in plasma sample was linear over the concentration range of 0.01-2.0 ${\mu}$g/mL. The intra- and inter-day assay accuracies of this method ranged from 86.82% to 108.33% of normal values and the precision did not exceed 13% of relative standard deviation. The plasma concentration of piroxicam decreased to below the quantifiable limit at 12 hr after the i.v. bolus administration to rabbits following dose of 0.375 mg/kg yielding a apparen t plasma half life of 1.38 hr. The transdermal route prolongs plasma levels of piroxicam. The bioavailability, calculated from the dose-adjusted ratio of the $AUC_{transdermal}$ to the $AUC_{i.v.}$, was 7.44%. The plasma concentration of piroxicam was detected by 48 hr after the transdermal administration of patch at a dose of 32 mg/kg. This method was suitable for cutaneous absorption studies of piroxicam in the rabbit after transdermal administration of different types of dosages of the drug.

• Journal of Pharmaceutical Investigation
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• 제30권4호
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• pp.279-282
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• 2000

Simple and precise high-performance liquid chromatographic (HPLC) assay was developed and validated for the determination of a HMG-CoA reductase inhibitor, $lovastatin^{TM}$ and its active metabolite (mevinolinic acid) in human plasma. The method involved solid phase extraction of mevinolinic acid and internal standard using Sep-Pak Cartridge. Samples were analyzed by reversed-phase HPLC using $Capcell-Pak\;C_{18}$ column with ultraviolet detection at 238 nm. The quantitation limit of mevinolinic acid was 2 ng/ml and the calibration curve was linear over the range of 2-50 ng/ml $(r^2>0.999)$ with human plasma. The analyses of quality control samples indicated that the normal values could be predicted with an accuracy >97%. The intra- and inter-day coefficients of variation for the analyses were <10%. The average recoveries were similar (79%) for mevinolinic acid and methylmevinolinic acid. The method described has been successfully applied to the quantification of mevinolinic acid in about 1,000 human plasma samples over six-month period.