• Title/Summary/Keyword: liquid-phase standard

Search Result 297, Processing Time 0.032 seconds

Liquid Chromatography-Tandem Mass Spectrometry for the Determination of Lithospermic Acid B in Rat Serum

  • Kim, Hui-Hyun;Ji, Hye-Young;Lee, Hye-Won;Kim, Youn-Chul;Sohn, Dong-Hwan;Lee , Hye-Suk
    • Archives of Pharmacal Research
    • /
    • v.27 no.12
    • /
    • pp.1202-1206
    • /
    • 2004
  • A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC-MS/ MS) method for the determination of lithospermic acid B (LSB) in rat serum was developed. LSB and internal standard, 7-hydroxy-3-phenyl-chromen-4-one (HPC) were extracted from rat serum with methyl-tert-butyl ether at acidic pH and analyzed on a Luna $C_8$ column with the mobile phase of acetonitrile-ammonium formate (10 mM, pH 6.5) (50:50, v/v). The analytes were detected using a negative electrospray ionization tandem mass spectrometry in the multiple- reaction-monitoring mode. The standard curve was linear $(r^2 = 0.997)$ over the concentration range of 10.0-500 ng/mL. The coefficient of variation and relative error for intra- and interassay at three QC levels were 1.1~6.2% and -10.3~-2.7%, respectively. The recovery of LSB from serum sample ranged from 73.2 to 79.5%, with that of HPC (internal standard) being 75.1 %. The lower limit of quantification for LSB was 10 ng/mL using 50 ${\mu}L$ of serum sample.

Simultaneous HPLC Analysis of Arachidonic Acid Metabolites in Biological Samples with Simple Solid Phase Extraction

  • Kim, Hyung-Gun;Huh, Young-Na;Park, Kun-Suk
    • The Korean Journal of Physiology and Pharmacology
    • /
    • v.2 no.6
    • /
    • pp.779-786
    • /
    • 1998
  • A reversed-phase high-performance liquid chromatogrphy (RP-HPLC) has been developed to analyze the metabolites of arachidonic acid based on the specificities of ultraviolet absorption of these various metabolites and is sensitive to the nanogram level. This procedure makes it possible to extract complex mixtures of eicosanoids efficiently with a single step and to analyze them simultaneously by RP-HPLC from biological samples using octadesylsilyl silica extraction column and $PGB_2$ as an internal standard. The cyclooxygenase products {prostaglandin $(PG)D_2,\;PGE_1,\;PGE_2,\;PGF_{1{\alpha}},\;PGF{2{\alpha}},\;6-keto-PGF_{1{\alpha}},$ and thromboxane $B_2(TXB_2)}$ and lipid peroxidation product, isoprostanes, of arachidonic acid were monitored by one isocratic HPLC system at 195 nm wavelength. The lipoxygenase products ${leukotriene(LT)B_4,\;LTC_4,\;LTD_4,$ and 5-hydroxyeicosatetraenoic acid (5-HETE), 12-HETE, 15-HETE} were measured by another isocratic HPLC system at 280 nm for LTs and 235 nm for HETEs. This method provides a simple and reliable way to extract and assess quantitatively the final arachidonic acid metabolites.

  • PDF

Determination of Nebramycin Factor 2,4,5,5',6 and Kanamycin A in Fermentation Broth of Streptoalloteichus hindustanus ATCC 31218 Mutant Using 2,4-Dinitrofluorobenzene(DNFB) as a Derivatizing Agent by High Performance Liquid Chromatography (HPLC법에 의한 2,4-디니트로플루오로벤젠을 유도체화제로 한 Streptoalloteichus hindustanus ATCC 31218 변이균의 배양액 중 네브라마이신 펙터 2,4,5,5',6, 가나마이신 A 분석)

  • 박영근;박명용;김승철;양호길
    • YAKHAK HOEJI
    • /
    • v.37 no.1
    • /
    • pp.1-8
    • /
    • 1993
  • A procedure for the high-performance liquid chromatographic determination of Nebramycin factors in fermentation broth of Streptoalloteichus hindustanus ATCC 31218 mutant was investigated using pre-column derivatization and LTV detection. The method is based on pre-column derivatization of Nebramycin factors with 2,4-dinitrofluorobenzene(DNFB) in the presence of Tris (hydroxymethyl)aminoethane. The chromatographic separation of derivatives of Nebramycin factors and unknown impurities is achieved using reversed-phase column (NOVA-PAK $C_{18}$, Waters Co.) and AcCN : H$_{2}$O : AcOH (53.0:46.5:0.5) as a mobile phase. The mixture of these derivatives were separated within 35 minutes and the optimum wavelength($\lambda_{max}$ ) of the UV detector was 353 nm. The linearity of response for derivatives of Nebramycin factors is demonstrated for concentrations up to 500 $\mu\textrm{g}$/ml and the relative standard deviation is less than 0.79%. Detection limit was 1.67 ng for the 10 $\mu\textrm{l}$ sample volume employed.

  • PDF

High Performance Liquid Chromatographic Determination of Ginseng Saponins (인삼 사포닌의 High Performance Liquid Chromatography에 의한 분리)

  • 홍순근;박은규;이춘영;김명운
    • YAKHAK HOEJI
    • /
    • v.23 no.3_4
    • /
    • pp.181-186
    • /
    • 1979
  • A high performance liquid chromatograpic procedure is described for determining ginseng saponins such as ginsenoside-Rb1, -Rb2, -Rc, -Rd, -Re, -Rf, -Rg1, and-Rg2. Ginseng saponins extracted with 90% methanol and water-saturated butanol were compared with pure standard ginsenosides. The resolution of the saponins was satisfactory and detection limit for each saponin was about 5.mu.g. Separation of the saponins was accomplished using a .mu. Bondapak carbohydrate analysis column, mobile phase of acetonitrile-water-butanol (80:20:15) and differential refractive index (RI) detector. The reproducibility and the recovery were also studied. This method was applied for determining the saponin contents of several parts of leaf, fresh ginseng, white ginseng, and red ginseng.

  • PDF

A Study on the Analytical Method of Trace Metal Ions in Sea Water by Inductively Coupled Plasma - Mass Spectrometry using Solid-Liquid Extraction Technique (유도결합 플라스마-질량분석법과 고체-액체 추출법을 이용한 해수중 미량금속의 분석에 관한 연구)

  • Lee, Won;Park, Kyung-Su;Kim, Eun Kyung;Hur, Young-Hoe
    • Analytical Science and Technology
    • /
    • v.11 no.6
    • /
    • pp.499-504
    • /
    • 1998
  • An analytical method for the simultaneous measurement of trace Cu, Sn, and Bi in sea water has been investigated by Inductively Coupled Plasma-Mass Spectrometry. Amberlite IRC-718 resin was used as a solid phase in solid-liquid extraction technique for the removal of matrix interferences such as Na, S, P, and other polyatomic ion species. Recoveries of 99.8% for Cu, 99.6% for Sn, and 97.9% for Bi were obtained for the standard spiked sample. The developed method was applied to analysis of trace metals in sea water.

  • PDF

Analysis of oligosaccharides from Panax ginseng by using solid-phase permethylation method combined with ultra-high-performance liquid chromatography-Q-Orbitrap/mass spectrometry

  • Li, Lele;Ma, Li;Guo, Yunlong;Liu, Wenlong;Wang, Yang;Liu, Shuying
    • Journal of Ginseng Research
    • /
    • v.44 no.6
    • /
    • pp.775-783
    • /
    • 2020
  • Background: The reports about valuable oligosaccharides in ginseng are quite limited. There is an urgent need to develop a practical procedure to detect and analyze ginseng oligosaccharides. Methods: The oligosaccharide extracts from ginseng were permethylated by solid-phase methylation method and then were analyzed by ultra-high-performance liquid chromatography-Q-Orbitrap/MS. The sequence, linkage, and configuration information of oligosaccharides were determined by using accurate m/z value and tandem mass information. Several standard references were used to further confirm the identification. The oligosaccharide composition in white ginseng and red ginseng was compared using a multivariate statistical analysis method. Results: The nonreducing oligosaccharide erlose among 12 oligosaccharides identified was reported for the first time in ginseng. In the comparison of the oligosaccharide extracts from white ginseng and red ginseng, a clear separation was observed in the partial least squares-discriminate analysis score plot, indicating the sugar differences in these two kinds of ginseng samples. The glycans with variable importance in the projection value large than 1.0 were considered to contribute most to the classification. The contents of oligosaccharides in red ginseng were lower than those in white ginseng, and the contents of maltose, maltotriose, maltotetraose, maltopentaose, maltohexaose, maltoheptaose, maltooctaose, maltononaose, sucrose, and erlose decreased significantly (p < 0.05) in red ginseng. Conclusion: A solid-phase methylation method combined with liquid chromatography-tandem mass spectrometry was successfully applied to analyze the oligosaccharides in ginseng extracts, which provides the possibility for holistic evaluation of ginseng oligosaccharides. The comparison of oligosaccharide composition of white ginseng and red ginseng could help understand the differences in pharmacological activities between these two kinds of ginseng samples from the perspective of glycans.

Radiological analysis of transport and storage container for very low-level liquid radioactive waste

  • Shin, Seung Hun;Choi, Woo Nyun;Yoon, Seungbin;Lee, Un Jang;Park, Hye Min;Park, Seong Hee;Kim, Youn Jun;Kim, Hee Reyoung
    • Nuclear Engineering and Technology
    • /
    • v.53 no.12
    • /
    • pp.4137-4141
    • /
    • 2021
  • As NPPs continue to operate, liquid waste continues to be generated, and containers are needed to store and transport them at low cost and high capacity. To transport and store liquid phase very low-level radioactive waste (VLLW), a container is designed by considering related regulations. The design was constructed based on the existing container design, which easily transports and stores liquid waste. The radiation shielding calculation was performed according to the composition change of barium sulfate (BaSO4) using the Monte Carlo N-Particle (MCNP) code. High-density polyethylene (HDPE) without mixing the additional BaSO4, represented the maximum dose of 1.03 mSv/hr (<2 mSv/hr) and 0.048 mSv/hr (<0.1 mSv/hr) at the surface of the inner container and at 2 m away from the surface, respectively, for a 10 Bq/g of 60Co source. It was confirmed that the dose from the inner container with the VLLW content satisfied the domestic dose standard both on the surface of the container and 2 m from the surface. Although it satisfies the dose standard without adding BaSO4, a shielding material, the inner container was designed with BaSO4 added to increase radiation safety.

Concentration and Seasonal Variation of Gaseous Nitrous Acid in Seoul Air (서울대기중 아질산기체의 계절별 농도변화)

  • 이용근;김종욱;이동수;백선영
    • Journal of Korean Society for Atmospheric Environment
    • /
    • v.10 no.1
    • /
    • pp.24-31
    • /
    • 1994
  • Hourly variation of gaseous nitrous acid( HNO$_2$) concentration in Seoul air was monitored from Jan. 11 to SeP. 12, Nitrous acid concentration was determined by DS/IC over nine months of observation, HNO$_2$ range from 0.04 ppb to 5.5 ppb. Gor-tex tube as gaseous HNO$_2$generator in this study is thought to be more convenient and reproducible device than previous generator. As a result of NaOH instead of Na$_2$ CO$_3$/NaHCO$_3$ solution as the IC eluent, we could obtain more stable baseline. The concentration of the NaOH eluent was 15 mM . The limit of detection(3$\sigma$) of the liquid- Phase and gas phase nitrous acid of this method are 1.1ng/$m\ell$ , 0.04 n $\ell$ / $\ell$, respectively. The precisions evaluated by 10 replicate analysis of standard solution and standard gas generated are $\pm$1.59, $\pm$2. 89% RSD, respectively. Due to the lack of standard material for air, direct assessment of the accuracy was not possible. This study was applied to the analysis of Seoul ambient air and their results are reported herein.

  • PDF

Optical Compensation of IPS-LCD for Symmetric-High-Contrast at Off-Axis Oblique View (측면시야각에서의 대칭적 명암대비비 향상을 위한 IPS-LCD 광학보상)

  • Kim, Tae-Hyeon;Kim, Bong-Sik;Park, Woo-Sang
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
    • /
    • v.29 no.3
    • /
    • pp.175-180
    • /
    • 2016
  • In this study, we proposed an optical compensation method to improve the symmetricity of contrast ratio for wide viewing angle IPS (in-plane switching) LCD. First, the phase retardation depending on the thickness of compensation film is calculated, and then the phase change is presented at the $Poincar{\acute{e}}$ sphere. The phase retardation and the polarization state of the light passing through the optical elements are caculated by using the EJMM (extended Jones matrix method). In addition, the transmittance and the contrast countour are also calculated by using the Berremann's $4{\times}4$ matrix method. The simulation is carried out for a IPS LC cell with positive A/C/A compensation film. From the standard deviation of the contrast ratio, we confirmed the symmetricity at each viewing angle is inversely proportional to the standard deviation and calculated the optimum design condition of the uniaxial compensation film for the IPS LCD.

Advanced Method for Determination of Omeprazole in Plasma by HPLC

  • Kang, Won-Ku;Kim, Dong-Sup;Kwon, Dwang-Il
    • Archives of Pharmacal Research
    • /
    • v.22 no.1
    • /
    • pp.86-88
    • /
    • 1999
  • An advance d and sensitive high-performance liquid chromatographic (HPLC) method for determination of omeparzole in human plasma has been developed. After omeprazole was extracted from plasma with diethylether, the organic phase was transferred to another tube and trapped back with 0.1 N NaOH solution. The alkaline aqueous layer was injected into a reversed-phase C8 column. Lansoprazole was used as an internal standard. The mobile phase consisted of 30% of acetonitrile and 70% of 0.2 M $ KH_{2}PO_{4}$, pH 7.0. Recoveries of the analytes and internal standard were >75.48%. The coefficients of variation of intra- and inter-day assay were <5.78 and 4.59% for plasma samples. The detection limit in plasma was 2 ng/ml. The clinical applicability of this assay method was evaluated by determining plasma concentration-time courses of the respective analytes in 24 healthy volunteers after oral administration 40 mg of omeprazole. The present assay is considered to be simple, accurate, economical and suitable for the study of the kinetic disposition of omeprazole in the body.

  • PDF