• 제목/요약/키워드: reversed phase

검색결과 606건 처리시간 0.023초

Quantitative Determination of Diterpenoids from the Roots of Aralia cordata

  • Lee, Mi-Kyoung;Hung, Tran Manh;Min, Byung-Sun;Lee, Ik-Soo;Na, Min-Kyun;Woo, Mi-Hee;Son, Jong-Keun;Kim, Young-Ho;Choi, Jae-Sue;Bae, Ki-Hwan
    • Natural Product Sciences
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    • 제15권1호
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    • pp.50-54
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    • 2009
  • A simple and reliable reversed phase HPLC method was developed to determine pharmacologically active compounds ent-continentalic acid, kaurenoic acid, and continentalic acid from the roots of Aralia cordata. Quantitative analysis of diterpenoids of A. cordata were performed by reverse phase C-18 column using a isocratic of acetonitrile : 0.1% trifluoroacetic acid(70:30) with UV detection at 205 nm. The correlation coefficients of each calibration curve of ent-continentalic acid, kaurenoic acid, and continentalic acid were 0.9987, 0.9983, and 0.9986, respectively. The detection limit of ent-continentalic acid, kaurenoic acid, and continentalic acid were $0.5{\sim}1.0\;{\mu}g/mL$, respectively. The contents of ent-continentalic acid (1), kaurenoic acid (2), and continentalic acid (3) of the roots of A. cordata collected from seventeen district markets in Korea were $0.09{\sim}0.75\;mg/g$, $1.09{\sim}5.43\;mg/g$, and $2.69{\sim}9.08\;mg/g$, respectively.

HPLC에 의한 동물성 수산식품 중의 Vitamin $D_3$와 그 관련물질 정량에 관한 연구 (Quantification of Vitamin $D_3$ and Its Derivatives in Marine Animal Foods by HPLC)

  • 김성진;김지수;조용계
    • 한국응용과학기술학회지
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    • 제10권2호
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    • pp.11-18
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    • 1993
  • Contents of vitamin $D_3$ and 25-OH-vitamin $D_3$ in marine animal products(20 species) were determined by HPLC. The isomers of vitamin D, $D_2$ and $D_3$, were not clearly separated on a reversed phase, ${\mu}$ Bonda Pak, with 20% methanol-acetonitrile, and on a normal phase, Zorbax SIL. with 0.4% isopropanol-hexane, but 25-OH-vitamin $D_2$ and-$D_3$ were separated on either ${\mu}$ Bonda Pak with 10% methanol-acetonitrile, or on Zorbax SIL with 2.2% isopropanol-hexane, respectively. Although levels of vitamin $D_3$ and 25-OH-vitamin $D_3$ varied remarkably according to species, their average value(fish : $l,l87{sim}36,007$ I.U/sample 100g, mussel : $58{\sim}1,706$ I.U/sample 100g, pickle: $1,208{\sim}79,358$ I.U/sample 100g) was greatly higher than that of meat($80{\sim}100$ I.U/sample 100g) and dairy products($400{\sim}800$ I.U/sample 100g). Fatty tissues of fish and pickled fish intestines contained high level of vitamin $D_3$ and 25-OH-vitamin $D_3$, while the clam and mussel known to have various kinds of sterol including ${\Delta}^7$-sterol showed very low levels of vitamin $D_3$ and its derivative.

Collisionless Magnetic Reconnection and Dynamo Processes in a Spatially Rotating Magnetic Field

  • Lee, Junggi;Choe, G.S.;Song, Inhyeok
    • 천문학회보
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    • 제41권1호
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    • pp.45.1-45.1
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    • 2016
  • Spatially rotating magnetic fields have been observed in the solar wind and in the Earth's magnetopause as well as in reversed field pinch (RFP) devices. Such field configurations have a similarity with extended current layers having a spatially varying plasma pressure instead of the spatially varying guide field. It is thus expected that magnetic reconnection may take place in a rotating magnetic field no less than in an extended current layer. We have investigated the spontaneous evolution of a collisionless plasma system embedding a rotating magnetic field with a two-and-a-half-dimensional electromagnetic particle-in-cell (PIC) simulation. In magnetohydrodynamics, magnetic flux can be decreased by diffusion in O-lines. In kinetic physics, however, an asymmetry of the velocity distribution function can generate new magnetic flux near O- and X-lines, hence a dynamo effect. We have found that a magnetic-flux-reducing diffusion phase and a magnetic-flux-increasing dynamo phase are alternating with a certain period. The temperature of the system also varies with the same period, showing a similarity to sawtooth oscillations in tokamaks. We have shown that a modified theory of sawtooth oscillations can explain the periodic behavior observed in the simulation. A strong guide field distorts the current layer as was observed in laboratory experiments. This distortion is smoothed out as magnetic islands fade away by the O-line diffusion, but is soon strengthened by the growth of magnetic islands. These processes are all repeating with a fixed period. Our results suggest that a rotating magnetic field configuration continuously undergoes deformation and relaxation in a short time-scale although it might look rather steady in a long-term view.

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2'-deoxyribonucleosides의 단일 및 다성분계의 비선형 흡착평형식 (Nonlinear Adsorption Isotherm of Single and Multi-Components of 2'-Deoxyribonucleosides)

  • 김룡매;한순구;최대기;노경호
    • Korean Chemical Engineering Research
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    • 제43권2호
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    • pp.230-235
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    • 2005
  • 2'-deoxyribonucleosides중에서 dUrd(2'-deoxyuridine), dGuo(2'-deoxyguanosine), dAdo(2'-deoxyadenosine)의 단일 및 다성분계의 흡착평형식을 동적방법으로 구하기 위해 물과 메탄올(90/10, vol%)을 이동상으로 하는 역상 액체 크로마토그래피를 사용하였다. 시료의 주입부피가 증가함에 따라서 체류시간이 짧아지고 피크가 삼각형 모양을 보여서, Langmuir 흡착평형식으로 가정하였다. PIM (pulsed-input method)에 의해서 Langmuir 흡착평형식의 매개변수를 구하고, 경쟁적인 다성분계의 흡착평형식을 사용하였다. 체류시간이 짧은 dUrd와 dGuo의 경우에서는 단일 및 다성분계에서 실험값과 계산값이 잘 일치하였지만, 가장 늦게 용출되는 dAdo에서는 비이상 비선형적인 특성으로 인해서 약간의 오차가 있었다.

Rapid Determination of Imatinib in Human Plasma by Liquid Chromatography-Tandem Mass Spectrometry: Application to a Pharmacokinetic Study

  • Yang, Jeong Soo;Cho, Eun Gi;Huh, Wooseong;Ko, Jae-Wook;Jung, Jin Ah;Lee, Soo-Youn
    • Bulletin of the Korean Chemical Society
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    • 제34권8호
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    • pp.2425-2430
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    • 2013
  • A simple, fast and robust analytical method was developed to determine imatinib in human plasma using liquid chromatography-tandem mass spectrometry with electrospray ionization in the positive ion mode. Imatinib and labeled internal standard were extracted from plasma with a simple protein precipitation. The chromatographic separation was performed using an isocratic elution of mobile phase involving 5.0 mM ammonium formate in water-5.0 mM ammonium formate in methanol (30:70, v/v) over 3.0 min on reversed-stationary phase. The detection was performed using a triple-quadrupole tandem mass spectrometer in multiple-reaction monitoring mode. The developed method was validated with lower limit of quantification of 10 ng/mL. The calibration curve was linear over 10-2000 ng/mL ($R^2$ > 0.99). The method validation parameters met the acceptance criteria. The spiked samples and standard solutions were stable under conditions for storage and handling. The reliable method was successfully applied to real sample analyses and thus a pharmacokinetic study in 27 healthy Korean male volunteers.

역상 액체크로마토그래피에 있어서 이성분과 삼성분 이동상에 대한 페놀류의 머무름 거동 (Retention Behavior of the Phenols on the Binary and Ternary Mobile Phases in Reversed-Phase Liquid Chromatography)

  • 오대섭;이선행;김수한;김상태
    • 대한화학회지
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    • 제30권4호
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    • pp.352-358
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    • 1986
  • 페놀류의 머무름 거동에 대한 실험적 관찰을 이성분용매인 MeOH-Water, ACN-Water, THF-Water와 삼성분용매인 MeOH-Water, ACN-Water, THF-Water계에서 수행했다. 이 머무름 거동의 데이타들로써 용매의 성분비에 따른 크기인자를 예측할 수 있는 선형방정식을 얻었다. 또 페놀류의 최적 분리에 적합한 MeOH-Water이성분 용매를 기준하여 이론적으로 용매세기가 같은 이성분과 삼성분용매를 사용했고 이 등용매세기하에서 시료에 대한 머무름 거동의 특이성 효과는 이성분용매계가 삼성분용매계보다 더 크게 나타났다.

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Chromotropic Acid를 착화제로 이용한 이온쌍 액체 크로마토그래피에 의한 붕소의 분리와 정량 (Determination of Boron by Ion Pair Liquid Chromatography with Chromotropic Acid)

  • 윤영자;유구용
    • 대한화학회지
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    • 제39권4호
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    • pp.288-293
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    • 1995
  • chromotropic acid (1,8-Dihydroxynaphthalene-3,6-disulfonic acid)를 착화제로 이용한 붕소에 대한 분리 정량을 이온쌍 액체 크로마토그래피로 연구하였다. 이동상$(MeOH\; 61{\%},\;H_2O\;39{\%}$, 인산완충용액 pH=8.5)에 tetrabutylammonium bromide를 첨가하므로서 붕소-chromotropic acid 착물과 chromotropic acid를 poly(styrene-devinylbenzene) 역상컬럼(PRP-1, 15 $cm{\times}4.6$ mm i.d.) 상에서 분리할 수 있었으며, 또한 시료 용액중에 0.1 M의 tetrabutylammonium bromide를 첨가하므로 붕소와 chromotropic acid간의 착물형성을 촉진시켜 감도를 높일수가 있었다. 0.5~1000 ${\mu}g/L$ 농도범위에서 좋은 직선성을 나타내었고 검출 한계는 0.5 ${\mu}g/L$ (S/N=2)이었다. 제안된 방법으로 시판용 시약, $Na_2SO_4,\; NaOH,\; KCl$에 있는 미량의 붕소를 정량하였다.

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Determination of Glimepiride in Human Plasma by Liquid Chromatography-Electrospray Ionization Tandem Mass Spectrometry

  • Kim, Ho-Hyun;Chang, Kyu-Young;Lee, Hee-Joo;Han, Sang-Beom
    • Bulletin of the Korean Chemical Society
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    • 제25권1호
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    • pp.109-114
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    • 2004
  • A sensitive method for quantitation of glimepiride in human plasma has been established using liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Glipizide was used as an internal standard. Glimepiride and internal standard in plasma sample was extracted using diethyl etherethyl acetate (1 : 1). A centrifuged upper layer was then evaporated and reconstituted with the mobile phase of acetonitrile-5 mM ammonium acetate (60:40, pH 3.0). The reconstituted samples were injected into a $C_{18}$ reversed-phase column. Using MS/MS in the multiple reaction monitoring (MRM) mode, glimepiride and glipizide were detected without severe interference from human plasma matrix. Glimepiride produced a protonated precursor ion ([M+H]$^+$) at m/z 491 and a corresponding product ion at m/z 352. And the internal standard produced a protonated precursor ion ([M+H]]$^+$) at m/z 446 and a corresponding product ion at m/z 321. Detection of glimepiride in human plasma by the LC-ESI/MS/MS method was accurate and precise with a quantitation limit of 0.1 ng/mL. The validation, reproducibility, stability, and recovery of the method were evaluated. The method has been successfully applied to pharmacokinetic studies of glimepiride in human plasma.

LiINbO3 기판의 분극반전을 이용한 5.5 GHz 대역 SSB 광변조기의 설계 및 제작 (Design and Fabrication of 5.5GHZ SSB optical modulator with polarization reversed structure)

  • 정우진;김우경;양우석;이형만;이한영;권순우
    • 한국광학회지
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    • 제17권2호
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    • pp.175-180
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    • 2006
  • 리튬나이오베이트 기판의 분극 반전 기술을 이용하여 5.5 GHz대역의 SSB(Single Sideband) 광변조기를 설계 및 제작하였다. 분극 반전을 통해 광이 인가받는 유효전계가 마흐젠더 두 도파로에서 $90^{\circ}$ 위상차를 갖도록 할 수 있었다. 제작된 광변조기는 5.8 GHz의 중심주파수로, 1.9 V DC 인가 시 약 33 dB의 USB 억제율을, -10.6 V 인가 시 약 25 dB의 LSB 억제율을 나타내었다. 또한 2.5 GHz의 대역폭에서 15 dB 이하의 Sideband 억제율을 보이고 있다.

High Performance Liquid Chromatographic Assay of a New Fluoroquinolone, LB20304, in the Plasma of Rats and Dogs

  • Seo, Mi-Kyeong;Jeong, Yi-Na;Kim, Hoon-Joo;Kim, In-Chull;Lee, Yong-Hee
    • Archives of Pharmacal Research
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    • 제19권6호
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    • pp.554-558
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    • 1996
  • High-performance liquid chromatographic method was developed for the determination or LB 20304 (compound 1) in the plasma of rats and dogs. The analyte was deproteinized with 1 volume of methanol and 1/2 volume of 10% zinc sulfate, and the supernatant was injected onto a reversed-phase HPLC column. The mobile phase was a mixture of 24 parts of acetonitrile and 76 parts of 0.1% trifluoroacetic acid. The flow rate was 1 ml/min, and the effluent was monitored by fluorescence detector at an excitation wavelength of 337 nm and an emission wavelength of 460 nm. The retention time of compound 1 was 6.3 min. The assay of compound 1 was linear over the concentration range of 0.2-100.mu.g/ml in the plasma of rats and dogs. The lower limit of quantification was 0.2.mu.g/ml using 100.mu.l of plasma with a 97-99% accuracy and a 12-14% precision. In the 0.5, 5, and 50.mu.g/ml quality control samples, the intra- and inter-day accuracy were 88-95% and 88-97%, whereas intra- and interday precision were 0.5-6.6% and 0.2-9.3%, respectively, in the plasma of rats and dogs. The recoveries were 68-71% independent of concentration and species in the plasma. No interferences from endogenous substances were observed. Taken together, the above HPLC assay method by deproteinization and fluorescence detection was suitable for the determination of compound 1 in the preclinical pharmacokinetics.

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