• 대한환경공학회지
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• 제36권6호
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• pp.387-395
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• 2014

본 연구에서는 SBSE 전처리 장치와 GC-MS/MS를 이용하여 합성 향물질 11종을 동시 분석할 수 있는 분석법을 개발하기 위해 흡착 bar의 교반시간, 교반속도, 시료수의 pH, 시료수 용량, 염석제 투입량 및 메탄올 주입량 변화 등 SBSE (stir bar sorptive extraction) 전처리 조건과 GC-MS/MS (gas chromatography/tandem mass spectrometry)의 기기조건을 다양하게 변화시켜 SBSE-GC-MS/MS를 이용한 분석법을 개발하였다. 11종의 합성 향물질들에 대한 검출한계(LOD)는 2.1~4.1 ng/L였으며, 정량한계(LOQ)는 6.6~12.9 ng/L였다. 수돗물, 낙동강 원수, 하수처리장 최종방류수 및 해수를 이용하여 시료수의 matrix 영향을 살펴본 결과, 11종의 합성 향물질들의 회수율 및 RSD의 경우 각각 88%~119% 및 0.8%~7.5%로 양호한 결과를 나타내어 시료수의 matrix 영향을 받지 않는 것으로 나타났다. 본 연구에서 개발된 SBSE-GC-MS/MS 분석법은 40 mL 정도의 적은 시료수량으로도 고감도 분석이 가능하며, 용매류를 사용하지 않기 때문에 분석자의 건강 및 환경친화적인 분석법이라는 장점뿐만 아니라 간편하고, 빠르며 자동화된 방법이라는 장점을 가진다.

• 청정기술
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• 제22권4호
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• pp.250-257
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• 2016

As an attempt to replacing petroleum-based chemicals with bio-based ones, synthesis of furfural from biomass-derived xylose attracts much attention in recent days. Conventionally, furfural from xylose has been produced via the utilization of highly corrosive, toxic, and environmentally unfriendly mineral acids such as sulfuric acid or hydrochloric acid. In this study, microwave-assisted biphasic reaction process in the presence of novel bio-based heterogeneous acid catalysts was developed for the eco-benign and effective synthesis of furfural from xylose. The microwave was irradiated for reaction acceleration and a biphasic system consisting of $H_2O$ : MIBK (1 : 2) was designed for continuous extraction of furfural into the organic phase in order to reduce the undesired side products formed by decomposition/condensation/oligomerization in the acidic aqueous phase. Moreover, sulfonated amorphous carbonaceous materials were prepared from wood powder, the most abundant lignocellulosic biomass. The prepared catalysts were characterized by FT-IR, XPS, BET, elemental analysis and they were used as bio-based heterogeneous acid catalysts for the dehydration of xylose into furfural more effectively. For further optimization, the effect of temperature, reaction time, water/organic solvent ratio, and substrate/catalyst ratio on the xylose conversion and furfural yield were investigated and 100% conversion of xylose and 74% yield of furfural was achieved within 5 h at $180^{\circ}C$. The bio-based heterogeneous acid catalysts could be used three times without any significant loss of activity. This greener protocol provides highly selective conversion of xylose to furfural as well as facile isolation of product and bio-based heterogeneous acid catalysts can alternate the environmentally-burdened mineral acids.

• 한국식품저장유통학회지
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• 제12권6호
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• pp.600-607
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• 2005

포도씨을 이용한 고부가가치의 포도씨유 제조기술 개발 및 시제품을 생산하기위해 먼저 일반 재배 및 유기농 재배 포도로부터 각각 수거된 포도씨의 수율, 및 기능성성분(지방산, 피토스테롤, 토코페롤, 총카테킨 및 4가지 카테킨 조성)의 차이를 측정하여 비교하였다. 다음, 용매추출법과 화학적 정제방법에의한 포도씨로부터 고품질의 포도씨유의 제조기술을 개발하고 시제품을 생산하한 결과는 다음과 같다. 일반 재배 및 유기농 재배 포도로부터 얻어진 포도씨유 및 추출물의 수율 그리고 기능성성분(지방산, 피토스테롤, 토코페롤, 총카테킨 및 4가지 카테킨류)의 함량을 측정한 후 비교한 결과 대체적으로 일반 재배 및 유기농 재배 포도씨의 기능성성분의 함량에는 큰 차이가 없었다. 건조포도씨(1.0톤)를 볶음처리 후 분쇄하여 노르말-헥산으로 탈지하고 얻은 포도씨 원유를 탈검($0.15\%$ 인산) 및 탈산($20\%$ NaOH 용액) 처리 후 수증기증류 장치($240^{\circ}C$, 2시간, 5 mmHg)를 이용하여 탈색, 탈향 및 탈취공정을 차례로 거치면서 고품질의 포도씨유의 제조기술을 확립하였으며, 아울러 그로부터 최종 포도씨유 제품(50kg, 수율: $5.0\%$/건조 포도씨)을 생산하였다.

• 공업화학
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• 제5권4호
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• pp.597-608
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• 1994

$(NH_4)_2SO_4$와 저품위 bauxite의 황산화 반응에 따라 얻어진 ammonium aluminium sulfate로부터 수열균일침전을 통해 무정형 alumina gel수화물 및 결정형 boehmite를 합성하고 이로 부터 고순도 $Al_2O_3$를 제조하는 새로운 공정 개발을 시도하였다. 이 공정은 ammonium aluminium sulfate용액 중의 Fe 성분을 제거하기 위한 용매추출공정과 정제된 ammonium aluminium sulfate용액으로부터 균일침전에 의한 Al 함유 침전물의 생성에 관한 것으로 이루어져 있다. 추출제 Alamine 336에 의한 적절한 용매추출조건은 shaking time 4분, 수상에 대한 유기상의 비 0.25였다. Urea를 이용한 수열균일 침전반응은 Al 함유용액 중의 Al에 대한 urea의 당량비 6.0의 조건에서 반응온도 $100^{\circ}C$ 이하에서는 무정형 alumina gel 수화물, $120^{\circ}C$ 이상 $150^{\circ}C$ 이하에서는 pseudo boehmite 그리고 $150^{\circ}C$ 이상에서는 결정형 boehmite가 합성되었다. 이 합성된 무정형 alumina gel 수화물은 소성시간 2시간, 소성온도 $1000^{\circ}C$ 이상에서 그리고 결정형 boehnite는 소성시간 2시간, 소성온도 $1250^{\circ}C$ 이상에서 ${\alpha}-Al_2O_3$로 전이되며 얻어진 ${\alpha}-Al_2O_3$의 순도는 99.97%의 고순도였다.

• 한국식품저장유통학회지
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• 제9권3호
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• pp.338-344
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• 2002

본 연구는 포도 거봉종의 종자와 과피 추출물의 지질과산화 억제 효과와 암세포들에 대한 세포 독성을 살펴보았다. 추출 온도를 달리하여 추출한 종자와 과피의 에탄올 추출물과 추출물에 대한 분획물들을 이용하여 지질과산화물의 억제효과를 측정한 결과, 종자 및 과피 에탄올 추출물 모두 온도변화에 따른 영향은 없는 것으로 나타났으며, 추출물의 농도가 증가할수록 지질과산화물의 감소효과가 증가하였다. 종자 추출물의 경우, 3$0^{\circ}C$에서 추출한 에탄올추출물이 20 $\mu\textrm{g}$/$m\ell$ 농도에서 60.1%, 분획물 중에서는 ethyl acetate 분획물이 71.2%의 지질과산화를 억제하였다. 과피 에탄올 추출물의 경우, 5$0^{\circ}C$에서 추출한 추출물이 20 $\mu\textrm{g}$/$m\ell$ 농도에서 48.1%, 분획물 중에서는 hexane 분획물이 44.4%의 지질과산화를 각각 억제하였다. 암세포 생육 억제 효과에서는 모든 암세포(MCF-7, Hep3B 및 A549)에서 포도 종자 및 과피 에탄올 추출물 및 분획물들이 1.00 $\mu\textrm{g}$/ML 농도에서 대부분 50% 이상의 생육 억제율을 보였으며, 암세포에 대한 생육 억제와 정상 세포에 대한 selectivity에서는 종자 에탄올 추출물과 과피 에탄을 추출물간의 유의적인 차이는 나타나지 않았다. 본 연구 결과, 거봉포도종자 및 과피의 에탄올 추출물들과 각 분획물은 지질과산화 억제 효과와 암세포들에 세포 독성이 캠벨종의 포도종자 및 과피에 비하여 낮은 활성을 나타내었다.

• Journal of Pharmaceutical Investigation
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• 제35권3호
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• pp.137-142
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• 2005

A rapid, selective and sensitive reversed-phase HPLC method for the determination of glipizide in human serum was validated and applied to the pharmacokinetic study of glipizide. Glipizide and internal standard, tolbutamide, were extracted from human serum by liquid-liquid extraction with benzene and analyzed on a Nova Pak $C_{18}\;60{\AA}$ column with the mobile phase of acetonitrile-potassium dihydrogen phosphate (10 mM, pH 3.5) (4:6, v/v). Detection wavelength of 275 nm and flow rate of 0.7 ml/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed glipizide concentration (500 ng/ ml) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-1000 ng/ml with correlation coefficient greater than 0.999. The lower limit of quantitation using 0.5 ml of serum was 10.0 ng/ml, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 82.6 to 105.0% for glipizide with overall precision (% C.V.) being 1.13-13.20%. The percent recovery for human serum was in the range of 85.2 93.5%. Stability studies showed that glipizide was stable during storage, or during the assay procedure in human serum. The peak area and retention time of glipizide were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of glipizide in human serum samples for the pharmacokinetic studies at three different laboratories, demonstrating the suitability of the method.

• Journal of Pharmaceutical Investigation
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• 제35권6호
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• pp.437-443
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• 2005

A rapid, selective and sensitive reversed-phase HPLC method for the determination of a major metabolite of terfenadine, fexofenadine, in human serum was developed, validated, and applied to the pharmacokinetic study of terfenadine. Fexofenadine and internal standard, haloperidol were extracted from human serum by liquid-liquid extraction with acetonitrile and analyzed on a $Symmetry^{TM}$ C8 column with the mobile phase of 1% triethylamine phosphate (pH 3.7)-acetonitrile (67:33, v/v, adjusted to pH 5.6 with triethylamine). Detection wavelength of 230 nm for excitation, 280 nm for emission and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fexofenadine concentration (50 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 10-500 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 10 ng/mL, which was sensitive enough for the pharmacokinetic studies of terfenadine. The overall accuracy of the quality control samples ranged from 95.70 to 114.58% for fexofenadine with overall precision (% C.V.) being 3.53-14.39%. The relative mean recovery of fexofenadine for human serum was 90.17%. Stability studies (freeze-thaw, short-term, extracted serum sample and stock solution) showed that fexofenadine was stable during storage, or during the assay procedure in human serum. However, the storage at $-70^{\circ}C$ for 4 weeks showed that fexofenadine was not stable. The peak area and retention time of fexofenadine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fexofenadine in human serum samples for the pharmacokinetic studies of orally administered Tafedine tablet (60 mg as terfenadine) at three different laboratories, demonstrating the suitability of the method.

• Journal of Pharmaceutical Investigation
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• 제35권4호
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• pp.265-271
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• 2005

A rapid, selective and sensitive reversed-phase HPLC method for the determination of etodolac in human serum was developed, validated, and applied to the pharmacokinetic study of etodolac. Etodolac and internal standard, ibuprofen were extracted from human serum by liquid-liquid extraction with hexane/isopropanol (95:5, v/v) and analyzed on a Luna C18(2) column with the mobile phase of 1% aqueous acetic acid-acetonitrile (4:6, v/v). Detection wavelength of 227 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed etodolac concentration $(1\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-40\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 0.05 ${\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.00 to 110.00% for etodolac with overall precision (% C.V.) being 1.08-10.11%. The percent recovery for human serum was in the range of 76.73-115.30%. Stability studies showed that etodolac was stable during storage, or during the assay procedure in human serum. The peak area and retention time of etodolac were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of etodolac in human serum samples for the pharmacokinetic studies of orally administered Lodin XL tablet (400 mg as etodolac) at three different laboratories, demonstrating the suitability of the method.

• Journal of Pharmaceutical Investigation
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• 제35권6호
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• pp.423-429
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• 2005

A selective and sensitive reversed-phase HPLC method for the determination of fenoprofen in human serum was developed, validated, and applied to the pharmacokinetic study of fenoprofen calcium. Fenoprofen and internal standard, ketoprofen, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Luna C18(2) column with the mobile phase of acetonitrile-3 mM potassium dihydrogen phosphate (32:68, v/v, adjusted to pH 6.6 with phosphoric acid). Detection wavelength of 272 nm and flow rate of 0.25 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed fenoprofen concentration $(2\;{\mu}g/mL)$ with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of $0.05-100\;{\mu}g/mL$ with correlation coefficients greater than 0.999. The lower limit of quantification using 1 mL of serum was $0.05\;{\mu}g/mL$, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 92.27 to 109.20% for fenoprofen with overall precision (% C.V.) being 5.51-11.71 %. The relative mean recovery of fenoprofen for human serum was 81.7%. Stability (freeze-thaw, short and long-term) studies showed that fenoprofen was not stable during storage. But, extracted serum sample and stock solution were allowed to stand at ambient temperature for 12 hr prior to injection without affecting the quantification. The peak area and retention time of fenoprofen were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of fenoprofen in human serum samples for the pharmacokinetic studies of orally administered Fenopron tablet (600 mg as fenoprofen) at three different laboratories, demonstrating the suitability of the method.

• Journal of Pharmaceutical Investigation
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• 제36권1호
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• pp.45-51
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• 2006

A rapid, selective and sensitive reversed-phase HPLC method for the determination of dipyridamole in human serum was developed, validated, and applied to the pharmacokinetic study of dipyridamole. Dipyridamole and internal standard, loxapine, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Nova Pak $C_{I8}$ column with the mobile phase of 40 mM ammonium acetate:methanol:acetonitrile (35:35:30)(v/v/v, pH 7.8). Detection wavelength of 280 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed dipyridamole concentration (50 ng/mL) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 2-2000 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 2 ng/mL, which was sensitive enough for pharmacokinetic studies of dipyridamole. The overall accuracy of the quality control samples ranged from 103.94 to 105.86% for dipyridamole with overall precision (% C.V.) being 4.60-11.49%. The relative mean recovery of dipyridamole for human serum was 97.64%. Stability studies showed that dipyridamole was stable during storage, or during the assay procedure in human serum. The peak area and retention time of dipyridamole were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of dipyridamole in human serum samples for the pharmacokinetic studies of orally administered Dimor tablet (75 mg as dipyridamole) at three different laboratories, demonstrating the suitability of the method.