• 제목/요약/키워드: Liquid phase plasma

검색결과 174건 처리시간 0.027초

Simple and Rapid Liquid Chromatography-Tandem Mass Spectrometry Analysis of Arctigenin and its Application to a Pharmacokinetic Study

  • Thapa, Subindra Kazi;Weon, Kwon-Yeon;Jeong, Seok Won;Kim, Tae Hwan;Upadhyay, Mahesh;Han, Yo-Han;Jin, Jong-Sik;Hong, Seung-Heon;Youn, Yu Seok;Shin, Beom Soo;Shin, Soyoung
    • Mass Spectrometry Letters
    • /
    • 제8권2호
    • /
    • pp.23-28
    • /
    • 2017
  • Arctigenin is the main active ingredient of Fructus Arctii, which has been reported with a variety of therapeutic activities including anti-cancer, anti-inflammation, anti-virus, and anti-obesity effects. In this study, a simple and sensitive liquid chromatography-tandem mass spectrometry (LC-MS/MS) method was developed and validated for the determination of arctigenin in rat plasma. The assay utilized a simple protein precipitation with methanol and the mobile phase consisted of 100% methanol and water containing 0.1% formic acid (65:35 v/v). Arctigenin and the internal standard (psoralen) were monitored using a positive electrospray turbo ionspray mode with multiple reaction monitoring transitions of m/z $373.2{\rightarrow}136.9$ and m/z $187.2{\rightarrow}130.9$, respectively, and total chromatographic run time was within 5 min. The lower limit of quantification (LLOQ) of arctigenin was 5 ng/mL in the rat plasma. The intra- and inter-day accuracy of arctigenin at LLOQ and matrix-matched quality control samples ranged 97.4 - 104.8% and 97.2 - 102.0%, respectively. The intra-day precision was within 4.80% and the inter-day precision was within 5.92%. Application of the present method was demonstrated through a pharmacokinetic study after intravenous and oral administration of arctigenin in male Sprague Dawley rats.

ANALYSIS OF THIN FILM POLYSILICON ON GLASS SYNTHESIZED BY MAGNETRON SPUTTERING

  • Min J. Jung;Yun M. Chung;Lee, Yong J.;Jeon G. Han
    • 한국표면공학회:학술대회논문집
    • /
    • 한국표면공학회 2001년도 추계학술발표회 초록집
    • /
    • pp.68-68
    • /
    • 2001
  • Thin films of polycrystalline silicon (poly-Si) is a promising material for use in large-area electronic devices. Especially, the poly-Si can be used in high resolution and integrated active-matrix liquid-crystal displays (AMLCDs) and active matrix organic light-emitting diodes (AMOLEDs) because of its high mobility compared to hydrogenated _amorphous silicon (a-Si:H). A number of techniques have been proposed during the past several years to achieve poly-Si on large-area glass substrate. However, the conventional method for fabrication of poly-Si could not apply for glass instead of wafer or quartz substrate. Because the conventional method, low pressure chemical vapor deposition (LPCVD) has a high deposition temperature ($600^{\circ}C-1000^{\circ}C$) and solid phase crystallization (SPC) has a high annealing temperature ($600^{\circ}C-700^{\circ}C$). And also these are required time-consuming processes, which are too long to prevent the thermal damage of corning glass such as bending and fracture. The deposition of silicon thin films on low-cost foreign substrates has recently become a major objective in the search for processes having energy consumption and reaching a better cost evaluation. Hence, combining inexpensive deposition techniques with the growth of crystalline silicon seems to be a straightforward way of ensuring reduced production costs of large-area electronic devices. We have deposited crystalline poly-Si thin films on soda -lime glass and SiOz glass substrate as deposited by PVD at low substrate temperature using high power, magnetron sputtering method. The epitaxial orientation, microstructual characteristics and surface properties of the films were analyzed by TEM, XRD, and AFM. For the electrical characterization of these films, its properties were obtained from the Hall effect measurement by the Van der Pauw measurement.

  • PDF

고속액체크로마토그래피 텐덤질량분석기법을 이용한 사람 혈장 내 소라페닙 농도분석법의 개발 및 검정 (Development and Validation of the Determination of Sorafenib in Human Plasma using Tandem Mass Spectrometry Coupled with Liquid Chromatography)

  • 박대진;이성곤;김우미
    • 생명과학회지
    • /
    • 제22권11호
    • /
    • pp.1456-1462
    • /
    • 2012
  • 소라페닙은 멀티카이네즈 억제제로서 신세포암, 전이성 간세포암 환자의 치료에 효과가 입증된 경구용 항암제이다. 이 연구의 목적은 고속액체크로마토그래피 텐덤질량분석기법(LC/MS/MS)을 이용하여 사람 혈장 내 소라페닙의 농도를 측정하는 효율적인 방법을 개발하고 한국식품의약품안전청(KFDA) 기준에 따라 분석법을 검정하는 것이다. 혈장시료($100{\mu}l$)에 내부표준물질인 chlorantraniliprole을 첨가한 후 이소프로필알콜과 에틸아세테이트로 구성(1:4, v/v)된 0.1% 포름산 함유 추출용액을 혼합하였다. 원심분리 후 상층액을 취하여 원심감압농축하였다. 잔사를 이동상에 재용해하고 Waters사의 역상 XTerra$^{TM}$ C18 칼럼(입자크기 $3.5{\mu}m$)을 장착한 고속액체크로마토그래피 장치에 주입하였다. 액체크로마토그래피는 0.1% 포름산과 10 mM 암모늄 포메이트를 함유한 버퍼용액과 메탄올, 아세토나이트릴을 각각 1:6:3으로 혼합한 용액을 이동상으로 사용하였으며 5분 내에 측정을 완료하였다. 분석대상 물질들은 텐덤질량분석기에서 electrospray 양이온 이온화($ES^+$) 검출방식으로 확인하였으며 소라페닙은 'm/z 465.2 ${\rightarrow}$ 252.5', chlorantraniliprole은 'm/z 484.4 ${\rightarrow}$ 286.2'으로 구성한 multiple reaction monitoring 방법을 사용하였다. 검정 결과, 2-5,000 ng/ml의 농도 구간에서 양호한 직선성($r^2$ > 0.99)과 정확도(90.7-103.9%), 정밀도(10% 이하)를 나타내었다. 새롭게 개발된 LC/MS/MS을 이용한 사람 혈장 내 소라페닙의 농도 측정법은 KFDA 기준을 만족하였으며, 기존의 방법에 비해 민감도가 높은 방법이었다.

High-performance liquid chromatographic assay and oral pharmacokinetics of new anti-HIV uracil derivatives, KR-V analogues, in rats

  • Lee, Youngmi;Heeok Shim;Seoungryong Yu;Hochul Shin;Moonkoo Chung;Jungkoo Roh
    • 한국응용약물학회:학술대회논문집
    • /
    • 한국응용약물학회 1998년도 Proceedings of UNESCO-internetwork Cooperative Regional Seminar and Workshop on Bioassay Guided Isolation of Bioactive Substances from Natural Products and Microbial Products
    • /
    • pp.123-123
    • /
    • 1998
  • A number of uracil derivatives have been developed as anti-AIDS drugs having a mechanism of inhibiting cellular reverse transcriptase. A simple and rapid assay technique for recently synthesized KR-V analogues was developed using a high-performance liquid chromatography, and oral pharmacokinetics was examined for assessing their oral bioavailabilites. Plasma samples were analyzed by reversed-phase HPLC using an ODS column with an ultraviolet detection system. All the analogues were eluted within 12 min and the LOQ was 15-30 ng/$m\ell$. The extraction recoveries were higher than 85%, except KR-V1039, 1068 and 1720 having ester group. This chromatic method was well applied to the kinetic studies for KR-V analogues. Among 16 analogues tested in the present work, the 6 compounds including KR-V1123, 1122, 1784, 1783, 1736 and 1700 were found to be bioavailable for oral administration to rats.

  • PDF

Preparation of Affinity Column Based on ZR4+ Ion forPhosphoproteins Isolation

  • Lee, Seon-Mi;Bae, In-Ae;Park, Jung-Hyen;Kim, Tae-Dong;Choi, Seong-Ho
    • 대한화학회지
    • /
    • 제53권3호
    • /
    • pp.279-285
    • /
    • 2009
  • This paper has described about preparation of $Zr^{4+}$ affinity column based on the poly(styrene-co- gly-cidyl methacrylate) prepared by emulsion polymerization of styrene and glycidyl methacrylate in order to isolate phosphopeptide. The $Zr^{4+}$ ions were introduced after the phophonation of an epoxy group on polymeric microspheres. The successful preparation of $Zr^{4+}$-immobilized polymeric microsphere stationary phase was confirmed through Fourier transform infrared spectra, optical microscopy, scanning electron microscopy, X-ray photoelectron spectra and inductively coupled plasma-atomic emission spectrometer. The separation efficiency for $Zr^{4+}$ affinity column prepared by slurry packing was tested to phosphonated casein and dephosphonated casein. The resolution time (min) of the phosphonated casein was higher than that of dephosphated casein for $Zr^{4+}$ affinity polymeric microsphere by liquid chromatography. This $Zr^{4+}$ affinity column can be used for isolation of phosphonated casein from casein using liquid chromatography.

셀레늄이 강화된 이스트에서 셀레늄 단백질의 분리 및 확인 (Separation and identification of selenoproteins in selenium-enriched yeast)

  • 김경미;박용남
    • 분석과학
    • /
    • 제26권6호
    • /
    • pp.357-363
    • /
    • 2013
  • Selenium-containing proteins were separated from selenium-enriched yeast (SEY) using Trizol$^{(R)}$ reagent followed by anion exchange (AE) chromatography. This method is simpler and less time consuming than electrophoresis. Five selenium containing proteins were identified by on-line AE HPLC-ICP/MS (high performance liquid chromatography-inductively coupled plasma/mass spectrometry). Each protein was enzymatically hydrolyzed to seleno-amino acids and separated with RP (reverse phase) HPLC for the identification of selenoproteins.

Frit 첨가량에 따른 PDP용 형광체의 특성 연구 (Characteristics of Phosphors for PDP with Frit Contents)

  • 정아름;김형준;최성철
    • 한국세라믹학회지
    • /
    • 제47권2호
    • /
    • pp.146-150
    • /
    • 2010
  • Because the plasma display panel has used red, green and blue(RGB) phosphors, it has suffer from two intrinsic problems; 1) the cell defect due to the lack of binding force between phosphor particles and 2) mis-discharge because of difference of electrical characteristics among RGB phosphors. In order to control the mechanical and electrical properties of RGB phosphors, frit with $ZnOB_2O_3-SiO_2-Al_2O_3$ system was added to RGB phosphor as sintering additive. The mechanical properties were increased by the amount of frit. The amount of frit under 5 wt% rarely affected dielectric constant. However, there was the limit of amount because of decreasing optical properties seriously; over 3 wt% in red, over 10 wt% in green and blue.

Loxoprofen sodium 제제(레녹스정)의 생물학적 동등성시험 (Bioequivalence Study of Loxoprofen Sodium in healthy Volunteers)

  • 최주영;유내춘;박민수;김경환
    • Biomolecules & Therapeutics
    • /
    • 제6권4호
    • /
    • pp.417-422
    • /
    • 1998
  • Loxoprofen sodium (sodium 2-[4-(2-oxocyclopentylmethyl)phenyl] propionate dehydrate) is a nonsteroidal antiinflammatory drug of $\alpha$-phenyl propionic acid derivative. To test the bioequivalence of loxoprofen, the pharmacokinetic parameters of new preparation of loxoprofen, LENOX was compared with LOXONIN as a reference drug. Fourteen healthy volunteers were entered to the stydy (Yonsei University College of Medicine, Severance Hospital IRB approval No. 9608). They were administered 60 mg of loxoprofen in 2$\times$2 cross-over design. There was one week of drug-free interval between doses. The blood sample was taken on schedule up to 8 hours, and the plasma concentration loxoprofen was measured by reverse phase high-performance liquid chromatography (HPLC) with UV-detector. There were no significant difference between two preparations when AUC, Cmax, and Tmax were compared by ANOVA. The mean differences of AUC, Cmax, and Tmax were within 20% of the reference drug: the values were 2.22,5.61, and 12.50%, respectively. The confidence limits of AUC and Cmax but not Tmax satisfied the bioequivalence criteria. These results suggest that the tested LENOX is bioequivalent to the reference drug.

  • PDF

Determination of bioavailability of tolperisone HCI by HPLC

  • Yang, Sang-In;Choi, Sun-Hee;Lee, Seung-Jin;Jang, Choon-Gon;Lee, Seok-Yong
    • 대한약학회:학술대회논문집
    • /
    • 대한약학회 2002년도 Proceedings of the Convention of the Pharmaceutical Society of Korea Vol.2
    • /
    • pp.241.1-241.1
    • /
    • 2002
  • Tolperisone hydrochloride is used as a muscle relaxant. Very few assay methods of tolperisone were reported. such as potentiometry. spectrophotometry and high performance thin layer chromatography. In addition. there is no report related to HPLC method to determine the tolperisone level in biological sample. In this study, A very sensitive reverse phase high performance liquid chromatographic (RP-HPLC) method for the determination of tolperisone HCI in plasma has been developed. (omitted)

  • PDF

Solid Phase Extraction of Celecoxib from Drug Matrix and Biological Fluids by Grafted Poly β-cyclodextrine/allyl Amine Magnetic Nano-particles

  • Kamari, Sahar;Panahi, Homayon Ahmad;Baimani, Nasim;Moniri, Elham
    • Korean Chemical Engineering Research
    • /
    • 제55권3호
    • /
    • pp.287-295
    • /
    • 2017
  • Using nanotechnology, magnetic nanoparticles of iron oxide were produced via co-precipitation method and followed modification with organic compounds. In the next step, functionalized monomer was provided via coupling ${\beta}$-cyclodextrine and allylamine onto modified magnetic nanoparticles. These nanoparticles were used to establish the adsorption rate of celecoxib. Magnetic nanoparticles are modified by (3-mercaptopropyl)trimethoxysilane. Nano-adsorbent was characterized by analytical and spectroscopic methods, such as Fourier transform infrared spectroscopy, elemental analysis, thermo-gravimetric analysis, and transmission electron microscopy (TEM). Laboratory parameters, such as the kinetics of adsorption isotherms, pH, reaction temperature and capacity were optimized. Finally, by using this nano-adsorbent in the optimized condition, extraction of celecoxib from biological samples as urine, drug matrix and blood plasma was carried out by high performance liquid chromatography with sensitivity and high accuracy.