• 제목/요약/키워드: Separation flow

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수치에 따른 결명자 주요 Anthraquinone의 함량분석 (Quantitative Analysis of Anthraquinones in Cassiae Semen by Processing Method)

  • 서창섭;김정훈;신현규;황석연;김병수
    • 생약학회지
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    • 제45권3호
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    • pp.200-208
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    • 2014
  • In this study, we performed quantification determination of four major components including aurantio-obtusin, emodin, chrysophanol, and physcion in the 70% ethanol extracts of non-processed Cassiae Semen and processed Cassiae Semen using a high-performance liquid chromatography coupled with photodiode array detector. The analytical column for separation of the 4 constituents used a Gemini $C_{18}$ column kept at $40^{\circ}C$ by the gradient elution with 1.0% (v/v) acetic acid in water and 1.0% (v/v) acetic acid in acetonitrile as mobile phase. The flow rate was 1.0 mL/min and the injection volume was $10{\mu}L$. The amount of aurantio-obtusin, emodin, chrysophanol, and physcion in non-processed Cassiae Semen were 0.07%, 0.02%, 0.25%, and 0.10%, respectively. The amount of aurantio-obtusin, emodin, chrysophanol, and physcion in processed Cassiae Semen were 0.04-0.14%, 0.01-0.03%, 0.02-0.42%, and 0.01-0.24%, respectively. Consequently, the optimal processing condition of Cassiae Semen for the improvements of amounts of four anthraquinone compounds was obtained by roasting at $240^{\circ}C$ for 15 min.

Electrochromic 막의 특성과 물질이동 방지막의 효과에 대한 연구 (Studies on the properties of electrochromic films and the effect of migration barrier)

  • 황하룡;백지흠;허증수;이덕동;임정옥;장동식
    • 한국진공학회지
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    • 제9권3호
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    • pp.221-226
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    • 2000
  • 졸겔법 및 진공증착법으로 $WO_3$$V_2O_5$ 박막을 제조하고, 리튬이온을 이용하여 전기변색 소자를 제작한 후 광학적 특성을 조사하였다. 측정결과 졸겔법으로 제조된 $WO_3$ 박막과 $V_2O_5$ 박막을 수증기 분위기에서 $500^{\circ}C$로 1시간 열처리한 경우 가장 우수한 투과율 변화량을 나타내었다. 정.역방향 동작을 거듭할수록 $WO_3$막의 텅스텐과 ITO막의 인듐이 상호 확산하는 것을 관찰할 수 있었으며 이를 방지하기 위해 수백 $\AA$의 텅스텐 박막을 ITO와 $WO_3$막 사이에 삽입한 결과, cyclic voltamogram의 peak의 감소량이 1/10 이하로 감소하였으며, 리튬이온의 흐름에 의한 인듐과 텅스텐의 이동을 효과적으로 방지할 수 있었다.

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진동 원편광 이색성 분광기를 사용한 키랄 에폭사이드의 광학순도 분석 (Determination of Enantiopurity of Chiral Epoxides by Vibrational Circular Dichroism Spectroscopy)

  • 이주현;이충영;김건중
    • 공업화학
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    • 제23권6호
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    • pp.577-582
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    • 2012
  • 진동 원편광 이색성(VCD; Vibrational Circular Dichroism) 분석기기를 사용한 키랄 유도체의 광학순도 분석을 수행하였다. 이 분석법을 통하여 광학이성체의 절대배위와 2% 이내의 오차 범위 내에서 %EE 값을 용이하게 측정할 수 있었다. 또한 VCD분석을 연속순환방식으로 시간 변화와 함께 수행하여 키랄화합물의 %EE 값을 측정하였다. ECH와 글리시돌 두 키랄 성분이 섞인 2성분 계에서 특별한 분리조작 없이 각 성분에 대한 농도 및 %EE 변화를 동시에 모니터링하는 것이 가능하였다. 본 연구에서 응용한 VCD 분석법은 반응 중의 반응 속도 등을 연속적으로 측정하는데 유용한 기법이며, 서로 다른 키랄 화합물이 혼합되어 있는 경우에 각각의 광학순도를 시간 변화와 함께 비파괴법으로 측정하기에 편리한 방법임을 확인하였다.

플랩이 부착된 특수타의 동유체력 제어효과에 관한 연구 (Control Effect of Hydro-kinetic Force of a Special Rudder attached Flap)

  • 김옥석;이경우;안영규
    • 한국항해항만학회지
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    • 제32권10호
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    • pp.771-776
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    • 2008
  • 선박에서 제어판의 역할은 운동을 제어하는데 목적이 있으며 이는 곧 조종성능을 결정하는 중요한 요소이다. 본 연구에서는 플랩타의 성능평가를 위하여 $Re=3.0{\times}10^4$에서 영각에 대응하는 플랩각에 따른 속도 및 에너지 분포를 2-프레임 그레이레벨 상호상관 PIV기법을 이용하여 비교 분석하였다. 또한 영각 10도와 20도에서 전통적인 단동타의 유동특성과 비교하여 플랩타의 성능특성을 평가하였다. 영각 10도에서는 양력, 영각 20도에서는 항력에 의한 측압력을 향상시킬 수 있었다. 영각 10도에서 플랩조작만으로 박리점과 경계층영역의 변화가 가능하였다.

Method development and validation of spectrophotometric and RP-HPLC methods for simultaneous estimation of spironolactone and furosemide in bulk and combined tablet dosage forms

  • Chavan, Rohankumar R.;Bhinge, Somnath D.;Bhutkar, Mangesh A.;Randive, Dheeraj S.;Salunkhe, Vijay R.
    • 분석과학
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    • 제34권5호
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    • pp.212-224
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    • 2021
  • The intent of the present work was to develop a simple, sensitive, accurate, precise, rapid and economical UV- spectrophotometric and reverse phase high pressure liquid chromatographic method for the simultaneous estimation of Spironolactone and Furosemide in bulk and combined tablet dosage forms. UV-Spectrophotometry was carried out by simultaneous equation method using 0.02 M potassium dihydrogen phosphate buffer pH 3.5: Acetonitrile (50:50) v/v as a solvent. The linearity range was 2-14 ㎍ mL-1 for Spironolactone and Furosemide with a correlation coefficient > 0.99. The chromatographic separation was achieved on 250 mm × 4.6 mm, hypersil BDS C18 column with particle size 5 ㎛, by using an isocratic mixture of 0.02 M potassium dihydrogen phosphate buffer pH 3.5: Acetonitrile: tert butyl methyl ether (49:50:1) v/v/v as a solvent at a flow rate of 1 mL min-1 and UV detection was carried out at 254 nm. The retention time were observed to be 3.666 and 6.661 minutes for Furosemide and Spironolactone respectively. The two developed methods were validated according to the ICH guidelines for accuracy, precision, linearity, LOD, LOQ and were found to be within the limits. It can be concluded that these two methods could be successfully used for the simultaneous estimation of Spironolactone and Furosemide in bulk and combined tablet dosage forms.

Marker compounds contents of Salvia miltiorrhiza Radix depending on the cultivation regions

  • Seong, Gi-Un;Kim, Mi-Yeon;Chung, Shin-Kyo
    • Journal of Applied Biological Chemistry
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    • 제62권2호
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    • pp.129-135
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    • 2019
  • Salvia miltiorrhiza Radix is cultivated in Korea and China and is traditionally used to treat cardiovascular diseases. In this study, we developed and validated a quantitative analysis method for S. miltiorrhiza Radix using high-performance liquid chromatography (HPLC). Identification was performed using ultra performance liquid chromatography-tandem mass spectrometry. For quantitative analysis, we used seven marker compounds. Separation conditions for HPLC were optimized using an ODS column with gradient conditions of 1% formic acid in distilled water and 1% formic acid in acetonitrile, with a flow rate of 0.8 mL/min and a detection wavelength of 280 nm. This method showed good linearity ($R^2=0.9998$), precision (relative standard deviation ${\leq}3.3%$), accuracy (recovery of 94.16-102.89%), limit of detection ($7.53{\mu}g/mL$), and limit of quantification ($23.71{\mu}g/mL$). This approach successfully quantified marker compounds in S. miltiorrhiza Radix. The individual marker compounds were identified by comparing the molecular masses and retention times with does standard compounds. Marker compound contents of S. miltiorrhiza Radix were investigated with different cultivation regions. Seven marker compounds were detected and quantified in all samples. Among them, salvianolic acid B showed the highest contents and it ranged from 4.13 to 7.15%. The salvianolic acid B content (7.15%) of marker compound was the highest in Bonghwa, and the tanshinone IIA content (1.90%) was the highest in Pohang. The results of marker compounds and developed method were intended to provide a favorable reference for the study of S. miltiorrhiza Radix from different regions of Korea.

Establishment and validation of an analytical method for quality control of health functional foods derived from Agastache rugosa

  • Park, Keunbae;Jung, Dasom;Jin, Yan;Kim, Jin Hak;Geum, Jeong Ho;Lee, Jeongmi
    • 분석과학
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    • 제32권3호
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    • pp.96-104
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    • 2019
  • Agastache rugosa, known as Korean mint, is a medicinal plant with many beneficial health effects. In this study, a simple and reliable HPLC-UV method was proposed for the quantification of rosmarinic acid (RA) in the aqueous extracts of A. rugosa. RA was selected as a quantification marker due to its easiness in procurement and analysis. The developed method involved chromatographic separation on a $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}m$) at room temperature. The mobile phase consisted of water and acetonitrile both containing 2 % acetic acid and was run at a flow rate of $1mL\;min^{-1}$. The method was validated for specificity, linearity, precision, and accuracy. It was specific to RA and linear in the range of $50-300{\mu}g\;mL^{-1}$ ($r^2=0.9994$). Intra-day, inter-day, and inter-analyst precisions were ${\leq}0.91%\;RSD$, ${\leq}1.40%\;RSD$, and 1.94 % RSD, respectively. Accuracy was 93.3-95.9 % (${\leq}1.21%\;RSD$). The method could be applied to three batches of bulk samples and three batches of lab scale samples, which were found to be $0.64({\pm}0.04)mg\;g^{-1}$ and $0.48({\pm}0.02)mg\;g^{-1}$ for the dried raw materials of A. rugosa. The results show that the proposed method can be used as a readily applicable method for QC of health functional foods containing the aqueous extracts of A. rugosa.

Milk Fat Substitution by Microparticulated Protein in Reduced-fat Cheese Emulsion: The Effects on Stability, Microstructure, Rheological and Sensory Properties

  • Urgu, Muge;Turk, Aylin;Unluturk, Sevcan;Kaymak-Ertekin, Figen;Koca, Nurcan
    • 한국축산식품학회지
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    • 제39권1호
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    • pp.23-34
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    • 2019
  • Fat reduction in the formulation of cheese emulsion causes problems in its flowability and functional characteristics during spray-dried cheese powder production. In order to eliminate these problems, the potential of using microparticulated whey protein (MWP) in cheese emulsions was examined in this study. Reduced-fat white-brined cheese emulsions (RF) with different dry-matters (DM) (15%, 20%, and 25% excluding emulsifying salt) were produced using various MWP concentrations (0%-20% based on cheese DM of emulsion). Their key characteristics were compared to full-fat cheese emulsion (FF). MWP addition had no influence on prevention of the phase separation observed in the instable group (RF 15). The most notable effect of using MWP was a reduction in apparent viscosity of RF which significantly increased by fat reduction. Moreover, increasing the amount of MWP led to a decrease in the values of consistency index and an increase in the values of flow behavior index. On the other hand, using high amounts of MWP made the emulsion more liquid-like compared to full-fat counterpart. MWP utilization also resulted in similar lightness and yellowness parameters in RF as their full-fat counterparts. MWP in RF increased glossiness and flowability scores, while decreased mouth coating scores in sensory analyses. Fat reduction caused a more compact network, while a porous structure similar to FF was observed with MWP addition to RF. In conclusion, MWP showed a good potential for formulation of reduced-fat cheese emulsions with rheological and sensorial characteristics suitable to be used as the feeding liquid in the spray drying process.

Development and validation of LC-MS/MS for bioanalysis of hydroxychloroquine in human whole blood

  • Park, Jung Youl;Song, Hyun Ho;Kwon, Young Ee;Kim, Seo Jin;Jang, Sukil;Joo, Seong Soo
    • Journal of Biomedical and Translational Research
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    • 제19권4호
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    • pp.130-139
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    • 2018
  • This study aimed to analyze a high-performance liquid chromatography (HPLC) separation using a pentafluorophenyl column of parent drug hydroxychloroquine (HCQ) and its active metabolite, desethylhydroxchloroquine (DHCQ) applying to determine bioequivalence of two different formulations administered to patients. A rapid, simple, sensitive and specific liquid chromatography-tandem mass spectrometry (LC-MS/MS) method has been developed and validated for bioanalysis of HCQ and its metabolite DHCQ in human whole blood using deuterium derivative $hydroxychloroquine-D_4$ as an internal standard (IS). A triple-quadrupole mass spectrometer was operated using electrospray ionization in multiple reaction monitoring (MRM) mode. Sample preparation involves a two-step precipitation of protein techniques. The removed protein blood samples were chromatographed on a pentafluorophenyl (PFP) column ($50mm{\times}4.6mm$, $2.6{\mu}m$) with a mobile phase (ammonium formate solution containing dilute formic acid) in an isocratic mode at a flow rate of 0.45 mL/min. The standard curves were found to be linear in the range of 2 - 500 ng/mL for HCQ; 2 - 2,000 ng/mL for DHCQ in spite of lacking a highly sensitive MS spectrometry system. Results of intra- and inter-day precision and accuracy were within acceptable limits. A run time of 2.2 min for HCQ and 2.03 min for DHCQ in blood sample facilitated the analysis of more than 300 human whole blood samples per day. Taken together, we concluded that the assay developed herein represents a highly qualified technology for the quantification of HCQ in human whole blood for a parallel design bioequivalence study in a healthy male.

An HPLC-UV-based quantitative analytical method for Chrysanthemum morifolium: development, validation, and application

  • Jung, Dasom;Jin, Yan;Kang, Seulgi;Lee, Heesoo;Park, Keunbae;Li, Ke;Kim, Jin Hak;Geum, Jeong Ho;Lee, Jeongmi
    • 분석과학
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    • 제32권4호
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    • pp.139-146
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    • 2019
  • A simple and reliable analytical method based on high-performance liquid chromatography-ultraviolet detection was established for the analysis of the flowers of Chrysanthemum morifolium (CM). Luteolin-7-O-glucoside (LU7G) was chosen as a target analyte considering its content, availability, and ease of analysis. Chromatographic separation of LU7G was achieved using a Phenomenex Gemini $C_{18}$ column ($250{\times}4.6mm$, $5{\mu}m$) run with a mobile phase consisting of 0.5 % acetic acid in water and 0.5 % acetic acid in acetonitrile at a flow rate of $1.0mL\;min^{-1}$. The detection wavelength and column temperature were set at 350 nm and $40^{\circ}C$, respectively. Method validation was performed according to the AOAC guidelines and the method was specific, linear ($R^2=0.9991$ for $50-300{\mu}g\;mL^{-1}$), precise (${\leq}3.91%$RSD), and accurate (100.1-105.7 %). The limits of detection and quantification were 3.62 and $10.96{\mu}g\;mL^{-1}$, respectively. The established method was successfully applied to determine the contents of LU7G in various batches of bulk CM extracts and labscale CM extract. The developed method is a readily applicable method for the quality assessment of CM and its related products.