• 한방비만학회지
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• 제20권2호
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• pp.97-108
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• 2020

Objectives: Ephedra sinica and Wolbigachul-tang which contains Ephedra sinica are used to treat obesity in Korean medicine. The aim of this study was to analyze the quantities of ephedrine alkaloids by high-performance liquid chromatography. Methods: The analysis was performed using a YMC-Triat C18 column with operating at 25℃, and UV detection at 210 nm. The mobile phase used a gradient flow with 0.1% H3PO4 in water and acetonitrile. Specificity, linearity, precision, accuracy, limit of detection, and limit of quantification were measured for validation anaylsis. This method was applied to analyze the quantities of ephedrine alkaloids in Ephedra sinica and Wolbigachul-tang. Results: The concentration per Ephedra sinica (gram) of ephedrine and pseudoephedrine in Ephedra sinica decoction are 4.74±0.22 mg and 2.19±0.10 mg, respectively and in Wolbigachul-tang decoction are 6.39±0.34 mg and 2.97±0.21 mg, respectively. The retention time of ephedrine was 23.6 min and that of pseudoephedrine was 25.8 min, and norephedrine and methylephedrine were not detected. Conclusions: In conclusion, analyzed the concentration of ephedrine alkaloids in Ephedra sinica and Wolbigachul-tang by the developed validation method.

• Journal of Ginseng Research
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• 제40권3호
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• pp.220-228
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• 2016

Background: Among the various ginseng strains, Shizhu ginseng is endemic to China, mainly distributed in Kuandian Manchu Autonomous County (Liaoning Province, China); however, not much is known about the compounds (especially saponins) in Shizhu ginseng. Methods: A rapid, sensitive, and reliable ultra-high performance liquid chromatography coupled with MS/MS (UHPLC-MS/MS) method was developed to separate and identify saponins in Shizhu ginseng. Results: The separation was carried out on a Waters ACQUITY UPLC BEH $C_{18}$ column ($100mm{\times}2.1mm$, $1.7{\mu}m$) with acetonitrile and 0.1% formic acid aqueous solution as the mobile phase under a gradient elution at $40^{\circ}C$. The detection was performed on a Micromass Quattro Micro API mass spectrometer equipped with electrospray ionization source in both positive and negative modes. Under the optimized conditions, a total of 31 saponins were identified or tentatively characterized by comparing retention time and MS data with related literatures and reference substances. Conclusion: The developed UHPLC-MS/MS method was suitable for identifying and characterizing the chemical constituents in Shizhu ginseng, which provided a helpful chemical basis for further research on Shizhu ginseng.

• 한국어병학회지
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• 제20권2호
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• pp.139-145
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• 2007

인체에 널리 사용되고 있는 Aspirin (ASA)을 양식 뱀장어 (Anguilla japonica) 약욕 또는 경구 투여한 다음 혈장 중의 ASA와 salicylic acid (SA)의 양을 HPLC로 측정하였다. 뱀장어 혈장은 0.2 M HCl과 0.2 M orthophosphoric acid로 산성화시킨 다음 acetonitrile과 혼합하여 ASA와 SA를 추출하였다. 2약제의 정량은 Novapak C18과 UV detector (237 nm)가 장착된 HPLC로 측정하였다. 이 때 이동상은 740 ㎖의 증류수, 900 ㎕의 orthophosphoric acid와 180㎖의 acetonitrile을 사용하였다. ASA, SA 및 내부 표준물질로 사용한 2-methylbenzoic acid (MBA)의 retention time은 각각 4.8분, 8.4분 및 11.4분이였으며, 측정한계 농도는 ASA가 0.05 ㎍/㎖, SA는 0.01 ㎍/㎖였다. 혈장으로 부터의 평균회수율은 ASA가 70.8-99.6%, SA는 95.2-100.3%였다. 뱀장어에 ASA를 약욕 (20 ppm) 또는 경구투여 (50 ㎎/kg BW) 한 다음 채취한 혈장을 시료로 이 방법으로 ASA와 SA의 양을 측정한 결과 단지 SA만 검출되어졌고, ASA는 검출되지 않았다. 이는 ASA가 혈장내에서 신속히 SA로 분해되기 때문으로 판명되었다. 또 ASA에 약욕시킨 경우에는 약욕 후 3시간후에 혈장내의 SA양이 최고치에 도달하였으며, 경구투여 한 경우에는 7일후에 최고치에 도달하였다. 한편 ASA를 투여한 다음 ASA 무첨가 수조에 수용한 결과 2투여 경로 모두 48시간 이후에는 SA가 0.02-0.03 ㎍/㎖이 검출되어 잔류의 문제도 거의 없었다. HPLC를 이용한 혈장내의 ASA와 SA의 검출법은 신속하며 정확한 방법으로 뱀장어 이외의 어류에도 활용 가능할 것으로 생각된다.

• 분석과학
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• 제22권3호
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• pp.191-200
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• 2009

이 연구는 소형방출챔버와 방출셀을 이용한 총휘발성유기화합물(TVOC) 방출시험결과의 상관성을 규명하여 방출셀을 이용한 액상 건축자재 오염물질 방출시험 방법을 정립하고 활용방안을 제시하기 위한 기초 자료를 확보하고자 수행되었다. 소형방출챔버와 방출셀을 이용한 액상 건축자재 방출시험을 실시하기 위해 방출시험 적합성 여부를 판단하고 최적조건을 확립하기 위하여 방출시험장치, 분석기기에 대한 성능평가를 실시하였다. 방출시험 장치인 소형방출챔버와 방출셀의 배경농도 청정도, 기밀도, 회수율, 분석장치인 열탈착장치 회수율 및 GC/MS 기기재현성, 방법검출한계(MDL) 등을 평가한 결과 방출시험장치와 분석기기의 조건은 안정적이고 재현성과 감도가 양호하여 액상 건축자재에서 방출되는 오염물질에 대한 측정 분석조건이 최적화되었음을 확인할 수 있었다. 페인트, 접착제, 실란트로 구성된 40개의 액상 건축자재를 대상으로 소형방출챔버와 방출셀을 이용하여 오염물질 방출시험을 실시한 결과 방출되는 총휘발성유기화합물의 농도는 소형 방출챔버와 방출셀에서 모두 대수정규분포(log normal distribution)하였으며 시험방법차이에 따른 방출량 분포의 차이는 크지 않았다. 또한 방출셀을 이용하여 오염물질 방출시험을 실시하였을 때, 소형방출챔버를 이용하였을 때보다 약 1.35~1.41배 높은 방출량을 나타내었으며 상관계수(r)가 약 0.91~0.97의 범위를 보여 높은 상관성이 있는 것으로 확인되었다.

• 공업화학
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• 제16권5호
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• pp.609-613
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• 2005

토종콩에 포함된 daidzein과 genistein을 초임계 $CO_2$와 아임계/초임계 $H_2O$를 이용하여 추출하였다. 추출액은 역상 고성능 액체 코토마토그래피(RP-HPLC)를 사용하여 분석하였다. 초임계 유체의 온도와 압력, 에탄올 농도의 변화에 따라서 비배당체의 체류시간, 체류인자, 컬럼효율, 컬럼의 선택도, 분리도를 비교하였다. 초임계 $CO_2$를 사용하였을 때, daidzein과 genistein의 추출특성은 온도와 에탄올농도의 영향을 주로 받았다. 아임계/초임계 $H_2O$를 사용하였을 때는 초임계 상태의 $400^{\circ}C$, 250 bar에서의 추출효율이 가장 우수하였다. 일반적으로 초임계 $CO_2$를 사용하는 경우, 초임계 $H_2O$에 비해서 약 10배 이상 비배당체의 추출수율이 증가하였다.

• 한국임상수의학회지
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• 제16권1호
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• pp.31-36
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• 1999

The aim of this study is to determine the phagocytosis-promoting factor(s) for feline peripheral blood polymorphonuclear cells (PMN) by culture supernatant from mono-nuclear cells (MNC) treated with egg white derivatives (EWD). The phagocytic activity of PMN was analyzed by a flow cytometry system. The EWD did not show direct effect on the phagocytic response of PMN. The phagocytic activity of PMN was enhanced by culture supernatant from MNC but not PMN treated with EWD. Therefore, it was suggested that the enhanced phagocytic activity of feline PMN could be mediated by humoral factor(s) released from MNC treated with EWD. Thus, the phagocytosis-promoting factor(s) in supernatant fraction from MNC culture treated with EWD were isolated by reverse phase high pressure liquid chromatography. The resulting supernatant fraction on 29.02 minutes of retention time showed high phagocytic activity of PMN. The molecular weight of this supernatant fraction was 16 to 18 kDa when analyzed by capillary electrophoresis. The isoelectric point was pH 5.76 when assessed by ion-exchange chromatography. These results suggest that EWD stimulates feline MNC to elaborate a phagocytosis-promoting factor, 16 to 18 kDa of molecular weight, which could be an important mediator for the enhancement of phagocytic activity of feline peripheral blood phagocytes. Further study will be needed to elucidate this phagocytic factor.

• Korean Chemical Engineering Research
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• 제47권5호
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• pp.593-598
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• 2009

정상경유에 등유 및 부생연료유를 인위적으로 혼합한 후, SPE 전처리 과정과 HPLC 분석을 통해 석유제품 내에 함유되어 있는 식별제의 정성 정량분석방법에 관해 연구하였다. SPE 전처리 과정에서 시료주입 후 15분에 분취된 시료에서 가장 높은 농도의 식별제가 분석되었다. 경유제품에 1 mg/L의 식별제를 혼입시킨 후, 전처리를 거쳐 HPLC로 분석한 결과 9.8분의 머무름시간에서 $1626.92mV{\cdot}sec$ 의 감도로 식별제가 분석되었으며, 또한 기존의 UV-Spectroscopy법으로 분석이 힘들었던 산성조건의 석유제품에서 식별제 분석이 가능하였다.

• 분석과학
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• 제30권2호
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• pp.102-111
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• 2017

Here we reported a methodology for identification of triacylglycerols (TAGs) and diacylglycerols (DAGs) in coix seed by preparative thin layer chromatography (prep-TLC) and non-aqueous reversed-phase liquid chromatography (NARP LC)-atmospheric pressure chemical ionization (APCI) tandem mass spectrometry (MS/MS). Lipid components were extracted from coix seed by reflux extraction using n-hexane for 3 hr. TAGs and DAGs in coix seed extract were effectively purified and isolated from matrix interferences by prep-TLC and then analyzed by LC-APCI-MS and MS/MS for identification. TAGs were effectively identified taking into consideration of their LC retention behavior, APCI-MS spectra patterns, and MS/MS spectra of $[DAG]^+$ ions. In MS/MS spectra of TAGs, diacylglycerol-like fragment $[DAG]^+$ ions were useful to identify TAGs with isobaric fragment ions. Based on an established method, 27 TAGs and 8 DAGs were identified in coix seed extract. Among them, 15 TAGs and 8 DAGs were for the first time observed in coix seed. Interestingly, some of TAGs isolated by prep-TLC were partly converted into DAGs through probably photolysis process during storing in room temperature. Thus, degradation phenomenon of TAGs should be considered in the quality evaluation and nutritional property of coix seed. LC-APCI-MS/MS combined with prep-TLC will be practical method for precise TAG and DAG analysis of other herbal plants.

• Journal of Pharmaceutical Investigation
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• 제35권5호
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• pp.375-381
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• 2005

A rapid and specific high-performance liquid chromatographic method was developed and validated for the simultaneous determination of prostaglandin $E_{1}\;(PGE_{1})$ and prostaglandin $E_{1}$ ethyl ester $(PGE_{1}-EE)$ in hairless mouse skin homogenate. The sample treatment procedure involved deproteination and precipitation by acetonitrile. $PGE_{1}$ and $PGE_{1}-EE$ in supernatant were separated in a reversed-phase C18 column without being interfered by other components present in hairless mouse skin homogenate. 9-Anthracenecarboxylic acid was used as an internal standard. The retention times of $PGE_{1}$, 9-anthracenecarboxylic acid and $PGE_{1}-EE$ were, 4.5, 9.5 and 18.0 min, respectively. The assay showed linearity from 1 to $40\;{\mu}g/ml$ for both $PGE_{1}$ and $PGE_{1}-EE$. Precision expressed as RSD ranged from 2.3 to 14.1 % for $PGE_{1}$ and 1.6 to 11.0% for $PGE_{1}-EE$. Accuracy ranged from 100.5 to 119.6 % for $PGE_{1}$ and from 98.0 to 103.7% for $PGE_{1}-EE$. This method was employed successfully to follow the time course of concentrations of $PGE_{1}$ and $PGE_{1}-EE$ in hairless mouse skin homogenate for stability study.

• Journal of Electrochemical Science and Technology
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• 제11권1호
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• pp.50-59
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• 2020

Birnessite-type manganese dioxide (δ-MnO₂) with hierarchical micro-/mesoporosity was synthesized via sacrificial graphene template approach under mild hydrothermal conditions for the first time. Graphene template was obtained by a surfactant (cetyltrimethylammonium bromide, CTAB) assisted liquid phase exfoliation (LPE) in water. A thin PEDOT:PSS (poly (3,4-ethylene dioxythiophene): poly (styrene sulfonate)) layer was applied to improve electrical conductivity and rate capability of MnO₂. The MnO₂ (535 F g^-1 at 1 A g^-1 and 45 F g^-1 at 10 A g^-1) and MnO₂/PEDOT:PSS nanocomposite (550 F g^-1 at 1 A g^-1 and 141 F g^-1 at 10 A g^-1) delivered electrochemical performances superior to their previously reported counterparts. An asymmetric supercapacitor, composed of MnO₂/PEDOT:PSS (positive) and Fe₃O₄/Carbon (negative) electrodes, provided a maximum specific energy of 18 Wh kg^-1 and a maximum specific power of 4.5 kW kg^-1 (ΔV= 2 V, 1M Na₂SO₄) with 85% capacitance retention after 1000 cycles. The graphene-templated MnO₂/PEDOT:PSS nanocomposite obtained by a simple and green approach promises for future energy storage applications with its remarkable capacitance, rate performance and cycling stability