• Analytical Science and Technology
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• v.30 no.1
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• pp.20-25
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• 2017

An analytical method for determining potential endocrine disruptors (bisphenol A, 2-chlorophenol, 2,4-dichlorophenol, 2,4,6-trichlorophenol, pentachlorophenol, p-t-butylphenol, p-pentylphenol, p-hexylphenol, p-t-octylphenol, p-heptylphenol, nonylphenol) by solid-phase extraction (SPE) and High Perfomance Liquid Chromatography(HPLC) equipped with fluorescence and variable wavelength detector has been developed. The SPE process for sample concentration was performed on a commercially available Oasis HLB cartridge packed with polymeric sorbents. The effect of elution solvent and elution volume on the recoveries of the analytes were investigated with HPLC. Average recovery of >85% was achieved with 60mg sorbents using 5mL of methanol as elution solvent. Phenolic compounds in canned drinks, beverages and water samples were surveyed by this proposed method.

• Bulletin of the Korean Chemical Society
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• v.35 no.9
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• pp.2625-2629
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• 2014

Platelets are anuclear discoid-shaped blood cells with key roles in human body. To understand the mechanisms of their activation process, it is required to have analytical imaging techniques capable of acquiring platelet images under fully hydrated conditions. Herein, for the first time, we demonstrate the capability of synchrotron-based transmission X-ray microscopy (TXM) to study platelets (resting and ADP activated) under hydrated and air-dried conditions. To confirm the biological imaging capability of TXM, fixed platelets were imaged and compared with whole mount electron microscopy (EM) images. TXM provided morphological information with sufficient spatial resolution with simple and quick sample preparation procedure. We also observed temporal changes during the platelet activation, which initially had a discoid shape (0 s), formed pseudopodia (30 s) and generated a network of fibrin (5 min). Our results clearly demonstrate the potential of TXM technique to study fully hydrated biological samples under in situ conditions.

• Analytical Science and Technology
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• v.37 no.4
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• pp.220-229
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• 2024

This study aims to developing a method for estimating pharmaceutical compounds within a monolith column using high-performance liquid chromatography (HPLC). The monolithic column was prepared using copolymerization of glycidyl methacrylate, co-ethylene dimethacrylate, and co-acrylic acid inside a borosilicate tube of specific dimensions a 60 mm borosilicate tube length with 1.5 mm and 3.5 mm inner and outer diameters, respectively. A UV Ultra violet source with a wavelength of 365 nm was used, and the polymerization process involved mixing glycidyl methacrylate, acrylic acid, ethylene dimethacrylate as a binder, and 2,2-dimethoxy-2-phenyl acetate phenone as an initiator in suitable solvents consisting of ethanol and 1-hexanol. The polymerization process formed the monolith column after 4 minutes, and subsequently, the epoxy groups were altered to diol groups using 0.2 M hydrochloric acid HCl, which were pumped through the column for 3 hours at a flow rate of 10 µL·min^-1. Various techniques, such as Scanning Electron Microscope SEM, Brunauer-Emmett-Teller BET, Fourier-transform infrared spectroscopy FT-IR and HNMR, were utilized to characterize and confirm the structure of the monolith. The prepared monolith was employed to estimate and identify the pharmaceutical compound of warfarin using high-performance liquid chromatography HPLC. The analytical curve of warfarin was linear in the range of 3 to 100 ㎍·mL^-1 with an r² value of 0.999. The detection and quantification limits were 0.932 and 2.788 ㎍·mL^-1, respectively. The molar absorptivity and Sandells sensitivity were 2.99138 × 10⁶ L·mol^-1·cm^-1 and 103.1 × 10^-3 ㎍·cm^-2, respectively.

• Analytical Science and Technology
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• v.33 no.1
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• pp.23-32
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• 2020

Methamphetamine (MA) is the most common and available drug of abuse in Korea and its primary metabolite is amphetamine (AP). Detection of AP derivatives, such as MA, AP, phentermine (PT), MDA, MDMA, and MDEA by the use of immunoassay screening is not reliable and accurate due to cross-reactivity and insufficient specificity/sensitivity. Therefore, the analytical process accepted by most urine drug-testing programs employs the two-step method with an initial screening test followed by a more specific confirmatory test if the specimen screens positive. In this study, a gas chromatography-mass spectrometric (GC-MS) method was developed and validated for confirmation of MA and AP in human urine. Urine sample (500 µL) was added with N-isopropylbenzylamine as internal standard and ethyl chloroformate as a derivatization reagent, and then extracted with 200 µL of ethyl acetate. Extracted samples were analysed with GC-MS in the SIM/ Scan mode, which were screened by Cobas c311 analyzer (Roche/Hitachi) to evaluate the efficiency as well as the compatibility of the GC-MS method. Qualitative method validation requirements for selectivity, limit of detection (LOD), precision, accuracy, and specificity/sensitivity were examined. These parameters were estimated on the basis of the most intense and characteristic ions in mass spectra of target compounds. Precision and accuracy were less than 5.2 % (RSD) and ±14.0 % (bias), respectively. The LODs were 3 ng/mL for MA and 1.5 ng/mL for AP. At the screening immunoassay had a sensitivity of 100% and a specificity of 95.1 % versus GC-MS for confirmatory testing. The applicability of the method was tested by the analysis of spiked urine and abusers' urine samples.

• Korean Chemical Engineering Research
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• v.58 no.2
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• pp.286-292
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• 2020

This study presents an angular-based measurement on three-dimensional paper-based analytical devices (3D-PADs) for quantitative detection of albumin without using an image analyzer. We demonstrate a simple quantitative and straightforward approach based on the angle of the discolored area as detection criteria. 3D-PADs are rapidly fabricated by the wax-printing and laminating process. The 3D-PADs are treated with citrate buffer and tetrabromophenol blue to react with albumin in a sample solution. Dropping sample solution into sample pad in the 3D-PAD, fluid flows toward the assay zone laterally and vertically by capillary action. We find that the change of angle of the discolored area correctly reflects the concentration of albumin and is reliable determinant for the measurement of the albumin concentration. It is the first demonstration of angular-based detection as a simple, inexpensive, and equipment-free approach for point-of-care diagnosis.

• Analytical Science and Technology
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• v.34 no.2
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• pp.68-77
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• 2021

Cannabis is one of the most abused drugs in Korea. The main psychoactive component in cannabis, Δ9-tetrahydrocannabinol, is metabolized to 11-nor-9-carboxy-Δ9-tetrahydrocannabinol (THCCOOH) and THCCOOH-glucuronide (THCCOOH-glu) in the human liver, whereby the amount of THCCOOH-glu found in urine is twice as high as that of THCCOOH. The analytical process adapted by the majority of urine drug-testing programs involves a two-step method consisting of an initial immunoassay-based screening test followed by a confirmatory test if the screening test result is positive. In this study, a qualitative gas chromatography-mass spectrometry (GC-MS) method was developed and validated for the detection of THCCOOH in human urine, where THCCOOH-glu was converted into THCCOOH by alkaline hydrolysis. For purification of the urine extract prior to instrumental analysis, high-speed centrifugation was used to minimize interference. In addition, an injection-port derivatization method using ethyl acetate and N,O-bis(trimethylsilyl)-trifluoroacetamide containing 1 % trimethylchlorosilane was employed to reduce the time required for derivatization, and an aliquot of the final solution was injected into the GC-MS. The method was validated by measuring the selectivity, limit of detection (LOD), and repeatability. The sensitivity, specificity, precision, accuracy, Kappa, F-measure, false positive, and false negative rate were determined by comparing the GC-MS results with those obtained using the immunoassay. The LOD was determined to be 0.32 ng/mL, while the repeatability was within 9.1 % for THCCOOH. Furthermore, a comparison study was carried out, whereby the screening immunoassay exhibited a sensitivity of 86.4 % and a specificity of 100 % compared to GC-MS. The applicability of the developed method was examined by analyzing spiked urine and forensic urine samples obtained from suspected cannabis abusers (n = 221).

• Analytical Science and Technology
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• v.23 no.5
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• pp.429-436
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• 2010

The present research evaluates the efficiency of mixed resins between anion exchange resin and active carbon. We expected synergic effect from advantages of both adsorbents. Especially, this research focused on the removal of high cencentrated perchlorate ion from demilitarization solution. The total amount of the adsorbed perchlorate ion is increased considerably with mixed resins between mono functional anion exchange resin and granular active carbon from a single adsorbent. Results demonstated that this process not only improve the efficiency of adsorbing perchlorate, but save the time, space and cost for treating perchlotrate waste solution, because of reducing organic contaminant removing process. The interference effects from coexisting anions are not significant and can successfully applied to real demilitarization sample.

• Analytical Science and Technology
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• v.26 no.1
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• pp.11-18
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• 2013

Perchlorate ($ClO{_4}^-$) is the material that is used as propellants of rockets and material of explosive as a form of ammonium perchlorate salts. Ammonium perchlorate solution of high concentration is recovered from expired rocket through demilitarization process by the water-jet method. If people take perchlorate in food and water, it interferes with adsorption of iodide which is the substance needed to synthesize thyroid hormone in the thyroid gland. It has an bad influence upon disturbing pregnancy and synthesis of growth hormone. So the effective method is necessary to remove perchlorate anion in water. By considering economic aspect, we studied effective desorption (regeneration) of perchlorate anion from adsorbent with studies on removal and adsorption of perchlorate anion. Desorption experiment was conducted as batch type. Depending on various conditions (concentration, pH, cation anion form) elution, we evaluated amount, efficiency of desorption(amount of adsorption/desorption ${\times}$ 100). Also, research confirmed the efficiency of mixed resins between anion exchange resin and activated carbon and expected synergic effect from advantages of both adsorbents.

• Analytical Science and Technology
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• v.9 no.4
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• pp.345-354
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• 1996

Algal(II) Multidentate N, O-Schiff base ligands, such as bis(salicylaldehyde) ethylenediimine(SED), bis(salicylaldehyde) propylenediimine(SPD), bis(salicylaldehyde) diethylenetriimine(SDT), bis (salicylaldehyde) triethylenetetraimine(STT) and bis(salicyl-aldehyde)tetraethylenepentaimine(STP) were prepared. Stepwise proton dissociation constants of the Schiff base were measured potentiometrically in ethanol and a mixture of 70% dioxane and 30% $H_2O$. The stability constants of copper(II)-Schiff base complexes were in the order of Cu(II)-SPD${\leq}$Cu(II)-SED~STT${\leq}$Cu(II)-STP. Oxidation-reduction process of the Cu(II)-Schiff base complexes was involved with one-electron reaction.

• Analytical Science and Technology
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• v.12 no.3
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• pp.218-223
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• 1999

A single use, screen-printed sensor for the measurement of liquid phase ethanol was developed and its electrochemical performance was investigated. Disposable type edthanol sensor was fabricated by serially screen printing the carbon paste, silverd pasted and insulator inlon a polyester substrate to pattern working and reference electrode sites and electrical contact. Alcohol dehydrogenase(ADH) or alcohol oxidase(AOD) together with appropriate electron transfer mediators was immobilized on the working electrode. To improve the sensitivity and reproducibility of carbon paste electrode, some pretreatment procedures were applied and their resultant electrochemical performance was examined. The disposable type electrochemical ethanol sensor developed in this study conveniently determines the ethanol in liquid samples such as blood and in fermentation process.