• Title/Summary/Keyword: Analytical reagent

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Evaluation of Variation Method to Improve the Sensitivity of Immunoradiometric Assay (면역방사계수측정법의 민감도 향상을 위한 변법의 평가)

  • Won-Hyun Kwon;Mi-Ji Kang;;Ji-Sol Park;Jung-In Kim;Kyung-Jae Lee
    • The Korean Journal of Nuclear Medicine Technology
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    • v.27 no.1
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    • pp.29-35
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    • 2023
  • Purpose The concentration of PSA (Prostate Specific Antigen) after radical prostatectomy in prostate cancer patients is a predictor of biochemical recurrence, and the AUA (American Urological Association) is defined as biochemical recurrence when the concentration of PSA is measured at 0.2 ng/mL or more, and when the concentration is measured at 0.2 ng/mL or more at the retest. This standard is also applied our hospital. In this laboratory, the PSA reagent using IRMA (Immunoradiometric Assay) is used, and the sensitivity at a very low value was not as good as the reagent used in the department of laboratory medicine. This study aims to increase the reliability of the results by improving the precision and sensitivity of very low values. Materials and Methods As a reagent for the study, PSA reagent using IRMA was used. As a method to improve the precision and sensitivity of very low values, a variation method on the serum volume(25 uL, 50 uL, 100 uL, 200 uL) was studied, and variation usefulness evaluation was conducted. The evaluation items were compared the results of precision, analytical sensitivity, recovery rate, dilution test, high-dose hook effect test, parallel test and very low concentration values(n = 20). Results The validation results were displayed in the order of 25 uL, 50 uL, 100 uL, 200 uL. As the serum volume increased, it was confirmed that CV (Coefficient of Variation)(%) improved. Analytical sensitivity(ng/mL) was 0.038, 0.041, 0.017, 0.015 and recovery rate(%) was 101±3, 101±3, 99±2, 97±4. very low concentration values(ng/mL) between each volume(n=20) were 0.135±0.068, 0.076±0.050, 0.048±0.034, 0.046±0.034. and high dose hook effect appeared as the serum volume increased. Conclusion Through the variation usefulness evaluation, it was confirmed that as the serum volume increased, the precision and sensitivity improved at very low concentration values. However, it is necessary to pay special attention to the occurrence of high-dose hook effect as the serum volume increases. In the case of tests that requires very low concentration values, it is thought that the reliability of the result will be increased if the variation method is properly used after the variation usefulness evaluation.

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A Study of Analytical Sensitivity on TDM Test Kit in Clinical Chemistry (약물검사 키트의 분석 민감도에 대한 연구)

  • Chang, Sang Wu;Kim, Nam Yong;Lee, Hee Gyung;Kim, Hyun Jung;Lee, Yun Jung;Jin, Ok Bae;Kim, Mi Gyung
    • Korean Journal of Clinical Laboratory Science
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    • v.36 no.2
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    • pp.127-130
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    • 2004
  • Analytical sensitivity on TDM test is the lowest concentration that can be distinguished from background noise. The aim of study was to evaluate analytical sensitivity that is also referred to as the lower limit of detection(LLD) about difference between zero calibrator and isotonic saline sample. We tested for 10 days with zero calibrators and 0.85% saline samples while running trilevel control samples under control. Raw data divided by two groups calculated mean and standard deviation from two sample populations and analytical sensitivity by ${\bar{X}}+2SD$. In comparison with isotonic saline samples and zero calibrators, there were significant differences in phenytoin, phenobarbital and vancomycin, etc. Especially analytical sensitivity on phenytoin is at the same level as the upper limit of analytical measurement range with $40{\mu}g/mL$. We think the cause of this is matrix interference. In conclusion, we were sure that standard protocol for analytical sensitivity as lower limit of analytical measurement range on TDM test must be measured with zero standard rather than an isotonic saline sample and type 1 reagent DW for reducing matrix effects within interactions between different materials in a mixture.

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PAMAM Dendrimers Conjugated with L-Arginine and γ-Aminobutyric Acid as Novel Polymeric Gene Delivery Carriers

  • Son, Sang Jae;Yu, Gwang Sig;Choe, Yun Hui;Kim, Youn-Joong;Lee, Eunji;Park, Jong-Sang;Choi, Joon Sig
    • Bulletin of the Korean Chemical Society
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    • v.34 no.2
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    • pp.579-584
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    • 2013
  • In this study, we synthesized functional dendrimer derivatives as nonviral gene delivery vectors. Poly(amidoamine) dendrimer (PAMAM, generation 4) was modified to possess functional amino acids to enhance gene transfection efficiency. PAMAM G4 derivatives conjugated with L-arginine (Arg) and ${\gamma}$-aminobutyric acid (GABA) showed higher transfection efficiency and lower cytotoxicity compared to the native PAMAM G4 dendrimer. The polyplex of the PAMAM G4 derivative/pDNA was evaluated using an agarose gel retardation assay and Picogreen reagent assay. Additionally, the MTT assay was performed to examine the cytotoxicity of synthesized polymers. All PAMAM G4 derivatives showed lower cytotoxicity than PEI25kD. Particularly, PAMAM G4-GABA-Arg displayed enhanced transfection efficiency compared to the native PAMAM G4 dendrimer.

Liquid chromatographic enantioseparation of several amino acids as nitrobenzoxadiazole derivatives on polysaccharide trisphenylcarbamate derived chiral stationary phases

  • Suraj Adhikari;Alisha Bhandari;Wonjae Lee
    • Analytical Science and Technology
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    • v.36 no.4
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    • pp.143-151
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    • 2023
  • Considering the greater role of α-amino acids in our daily lives, the enantiomer resolution of seven α-amino acids derivatized with fluorogenic reagent (4-fluoro-7-nitro-2,1,3-benzoxadiazole, NBD-F) by chiral HPLC on amylose or cellulose trisphenylcarbamate derived chiral stationary phases (CSPs) under simultaneous ultraviolet (UV) and fluorescence (FL) detection was performed. The degree of enantioseparation and resolution was affected by nature and selector backbones of the CSPs as well as the kind of amino acids. Baseline enantiomer separation and resolutions were observed for the enantiomers of all analytes as NBD derivatives especially on coated type amylose tris(3,5-dimethylphenylcarbamate) derived CSPs (Chiralpak AD-H and Lux Amylose-1). The other CSPs also showed good enantioselectivity except for the CSPs (Chiralpak IB, Chiralcel OD-H and Lux Cellulose-1) having cellulose tris(3,5-dimethylphenylcarbamate) as chiral selectors. The developed analytical chiral method was applied to determine the enantiomeric purity of seven commercially available L-α-amino acids and the impurities as D-forms were found to be in the range 0.08-0.87 %, respectively. The intra- and interday accuracy and precision assays showed high accuracy and precision of the developed analytical method. This chiral HPLC method for the enantiomer resolution of amino acids using fluorescent derivatization could be useful for the determination of enantiomeric purity of pharmaceuticals and biological study for amino acid type compounds among chiral drugs.

Synthesis of Thiocatechols and Acid Dissociation Constants (Thiocatechol 및 그 유도체의 합성과 산해리 정수)

  • Oh, Joon-Suk;Lee, Kwang-Woo;Kim, Tek-Jae
    • Journal of the Korean Chemical Society
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    • v.12 no.1
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    • pp.1-3
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    • 1968
  • New chelating ligands, thiocatechol and p-chlorothiocatechol, have been synthesized and the acid dissociation constants were determined by potentiometric method in 50% dioxane-water; $pK_1 \;and\; pK_2$ were 7.28, 10.97 for thiocatechol and 6.37, 10.22 for p-chlorothiocatechol, respectively. Color reactions with various metal ions were studied. It was found that the above ligands are specific for Bi(III), Mo(VI) and W(VI) as an analytical reagent.

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Sensitive and Mild Fluorogenic Reagents for Biogenic Carboxylic Acids in HPLC

  • Ushijima, Tamano;Saito, Mikihiko;Sasamoto, Kazumi;Ohkura, Yosuke;Ueno, Keiyu
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.545-551
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    • 1995
  • Five acid hydrazides as precolumn fluorescence derivatization reagents for carboxylic acids in HPLC, which have the benzofuran or benzothiazole moiety conjugated to a furan, thiophene or oxazoline ring, were synthesized and examined in view of reactivity, separability and sensitivity. Of these hydrazides, 2-(5-hydrazinocarbonyl-2-oxazolyl)-5,6-dimethoxybenzothiazole (BTOH) was most favorable. The detection limit of lauric acid as a model acid was 0.1 pmol per $10-{\mu}l$ injection volume at S/N=3, which was roughly equal to that of an analogous compound, 2-(5-hydrazinocarbonyl-2-furyl)-5,6-dimethoxybenzothiazole. The reagent allowed rapid assays of carboxylic acids ($C_{12:0}-C_{20:4}$) within 20 min with satisfactory scparability. The method was applied to the determination of fatty acids in human sera from healthy volunteers as well as from patients with diabetes or thyroid dysfunction.

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Spectrophotometric Determination of Nickel in Steel with Di-2-pyridylmethanone 2-Thiophenecarboxylic Hydrazone

  • Nakanishi, Tsutomu
    • Analytical Science and Technology
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    • v.8 no.4
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    • pp.469-475
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    • 1995
  • Di-2-pyridylmethanon 2-thiophenecarboxylie hydrazone(DPMTCH) was synthesized and used as a chromogenic reagent in the spectrophotometric determination of nickel in steel. The proton disc spectrophotometrically, were $pK_{a1}= 2.66$ and $pK_{a2}= 10.98$ ${\mu}=0.5(NaCl)$. Nickel(II) reacts with DPMTCH to form a 1:2 metal-2-ligand ratio complex, the xylene solution of which has an absorption maximum at 417 nm. Beer's law is obeyed over the range $0-1.17\;mg\;ml^{-1}$ of nickel(II). The molar absorptivity of the nickel(II) complex is $4.17{\times}10^4l\;mol^{-1}\;cm^{-1}$. The precision of the method was estimated for 4.7 mg of nickel(II), the coefficient of variation for 15 replicate determinations being 0.34%.

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Numerical Analysis of Solid Propellant Ignition ~Numerical Formulation Assessment~

  • Shimada, Toru;Novozhilov, Boris V.
    • Proceedings of the Korean Society of Propulsion Engineers Conference
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    • 2004.03a
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    • pp.528-531
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    • 2004
  • For a simple one-dimensional ignition problem a mathematical model is described to investigate the difficulties in numerical simulations. Some computation results are obtained and comparison is made with analytical solution. Discussions are made on topics such as 1) coordinate transformation, 2) gas-phase and solid-phase analysis; (divergence form of the governing system, a finite-volume discretization, implicit time integration, upwind split flux, spatial accuracy improvement are described. Mass, reagent mass, and energy conservations are solved.), and 3) method to determine quantities on the burning surface (matching). Results obtained for small values of the non-dimensional pressure show a steady-combustion and good agreement with the analytical solution. Numerical instability appeared for larger values of the pressure, discussion on the cause of the problem is made. This effort is a part of a study of flame spread phenomena on solid propellant surface.

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Problem-solving approach for salbutamol analysis by HPLC during pharmaceutical assay

  • Gholizadeh-Hashjin, Aiesheh;Hamishehkar, Hamed;Monajjemzadeh, Farnaz
    • Analytical Science and Technology
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    • v.35 no.5
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    • pp.189-196
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    • 2022
  • When cationic basic compounds are chromatographed using hydro-organic mobile phase, the presence of anionic free silanols in the silica-based stationary phases results in broad and asymmetrical peaks. The addition of an ionic reagent to the mobile phase prevents analytes from accessing free silanols, improving peak shape. In this study, the chromatographic behavior of salbutamol sulfate as a basic compound was investigated under various conditions, including the use of different columns, mobile phases, and ion-pair reagents such as triethanolamine (TEA) and sodium heptane sulfonate (SHS). The retention and peak shape of chromatograms were both evaluated. The results show that pre-conditioning the column with TEA and including it in the mobile phase can prevent cationic analytes from accessing anionic silanols, resulting in improved peak shape. Furthermore, buffering the mobile phase is an important factor in keeping the pH constant throughout the process. The chosen method was validated in part. This study could be helpful for researchers and analyst to solve such problems with cationic basic components.

Determination of the Impurities in Isoprene by GC/MS (GC/MS를 이용한 이소프렌 중 불순물 분석)

  • Lee, Hyunjoo;Ahn, Byoung Sung;Suh, InSuk;Kwon, Young Soo
    • Analytical Science and Technology
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    • v.14 no.4
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    • pp.300-305
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    • 2001
  • The impurities in isoprene were determined using GC/MS. There were good linearities (above $R^2=0.996$) in the range of the $1.0-50{\mu}g/mL$ and 0.5-5.0%, and the detection limits of the method were below $0.1{\mu}g/mL$ for each impurities. Reagent-grade isoprene contained isopropenyl acetylene and 2-butyne at $10-50{\mu}g/mL$ and the concentrations of cis-piperylene, trans-piperylene, cyclopentadiene and dicyclopentadiene were below $1{\mu}g/mL$. The analysis confirmed that the reagent grade isoprene could be obtained from the distillation of C5 fractions.

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