• Analytical Science and Technology
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• v.14 no.6
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• pp.499-503
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• 2001

A new simple, rapid and sensitive gas chromatographic technique for the determination of bisphenol-A in can materials, which is the major material of epoxy resin and polycarbonate polymer, is proposed. This method is characterised by derivatization of the bisphenol-A with a acylating reagent forming the acetate derivative to optimize the chromatographic property. The detection of bisphenol-A is performed based on GC/MS (gas chromatography/mass spectrometry). Several beverages were analyzed by the proposed method for the determination of bisphenol-A Bisphenol-A was assayed the range of $0.11{\sim}11.40{\mu}g/can$ from the can materials.

• Analytical Science and Technology
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• v.24 no.1
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• pp.15-23
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• 2011

An accurate mass and isotope ratio were determined using a gas chromatography/time of flight mass spectrometer in CI positive mode for the identification of unknown metabolites. High mass tune was used to improve the ion intensity of $[M+H]^+$. Chromatographic resolution and dynamic range enhancement were performed to obtain more reliable accurate masses and correct isotope abundance ratios. Average absolute errors of mass and isotope ratios for 24 reference metabolite -TMS (trimethylsilyl) derivatives were 6.8 ppm, 1.5% of (M+1/M ratio) and 1.7% of (M+2/M ratio), respectively. The correct formulas of twenty one compound were retrieved within top-2 hit from the heuristic algorithm for elemental composition using each accurate mass and isotope abundance ratio.

• Analytical Science and Technology
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• v.32 no.5
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• pp.163-172
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• 2019

Methamphetamine (MA) is currently the most abused illicit drug in Korea and its major metabolite is amphetamine (AP). As MA exist as two enantiomers with the different pharmacological properties, it is necessary to determine their respective amounts in a sample. Thus a chiral stationary phase liquid chromatography-tandem mass spectrometric (LC-MS/MS) method was developed for identification and quantification of d-MA, l-MA, d-AP, and l-AP in human urine. Urine sample ($200{\mu}L$) was diluted with pure water and purified using solid-phase extraction (SPE) cartridge. A $5-{\mu}L$ aliquot of SPE treated sample solution was injected into LC-MS/MS system. Chiral separation was carried out on the Astec Chirobiotic V2 column with an isocratic elution for each enantiomer. Identification and quantification of enantiomeric MA and AP was performed using multiple reaction monitoring (MRM) detection mode. Linear regression with a $1/x^2$ as the weighting factor was applied to generate a calibration curve. The linear ranges were 25-1000 ng/mL for all compounds. The intra- and inter-day precisions were within 3.6 %, while the intra- and inter-day accuracies ranged from -5.4 % to 11.8 %. The limits of detection were 2.5 ng/mL (d-MA), 3.5 ng/mL (l-MA), 7.5 ng/mL (d-AP), and 7.5 ng/mL (l-AP). Method validation parameters such as selectivity, matrix effect, and stability were evaluated and met acceptance criteria. The applicability of the method was tested by the analysis of genuine forensic urine samples from drug abusers. d-MA is the most common compound found in urine and mainly used by abusers.

• Journal of Convergence for Information Technology
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• v.11 no.2
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• pp.107-116
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• 2021

In this study, an analytical method was developed for estradiol-17��, testosterone, and progesterone, which are growth promoters as veterinary drug residues in animal food. The analytes were separated using liquid chromatography, and was injected into a mass spectrometer through the electrospray ionization(ESI) process and detected in multiple reaction monitoring(MRM) mode. As the method was validated by CODEX CAC/GL 71-2009 guideline, it met the acceptable. The analysis of beef, pork, and chicken distributed in Korea was conducted with an established method to confirm the applicability of the actual sample. It was confirmed that the developed method can be quickly and reliably in the analysis for the growth promoters identified in domestic distributed livestock products. Through subsequent research, a highly utilized analysis method will be completed if the number of growth promoters is expanded based on the method and the simultaneous analytical method is established by including all of it.

• Structural Engineering and Mechanics
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• v.81 no.3
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• pp.305-316
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• 2022

Externally bonded ultrahigh performance fiber-reinforced concrete (UHPFRC) is commonly used as a strengthening material for reinforced concrete (RC) structures. This study reports the results of an experimental program investigating the bonding behavior between concrete and prefabricated UHPFRC plates. The overall experimental program is consisting of five RC specimens, which are strengthened using the different lengths and widths of prefabricated UHPFRC plates. These specimens were analyzed using the pull-pull double-shear test. The performance of each strengthened specimen is presented, discussed and compared in terms of failure mode, maximum load, load-slip relationship, fracture energy and strain distribution. Specimen C-25-160-300 which bonded along the whole width of 160 mm recorded the highest maximum load (109.2 kN) among all the analysed specimens. Moreover, a 3D numerical finite element model (FEM) is proposed to simulate the bond behavior between concrete and UHPFRC plates. Moreover, this study reviews the analytical models that can predict the relationship between the maximum bond stress and slip for strengthened concrete elements. The proposed FEM is verified against the experimental program and then used to test 36 RC specimens strengthened with prefabricated UHPFRC plates with different concrete grades and UHPFRC plate widths. The obtained results together with the review of analytical models helped in the formation of a design equation for estimating the bond stress between concrete and prefabricated UHPFRC plates.

• Analytical Science and Technology
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• v.21 no.2
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• pp.84-92
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• 2008

A method for the determination of trace amount of caffeine in urine and various drink samples using hollow fiber-liquid phase microextraction (HF-LPME) and capillary gas chromatograph/nitrogen phosphorus detector (GC/NPD) has been established. HF-LPME method has been optimized with respect to several experimental parameters including the effects of the hollow fiber length, extraction solvent, stirring mode, pH and salt concentration for the determination of caffeine from aqueous samples. The correlation coefficient of calibration curve for caffeine was 0.9994. The average recovery was 102%(n=3). The established method is feasible for the determination of trace amounts of caffeine in several aqueous sample. The limit of detection (LOD) and the limit of quantitation (LOQ) have been found to be 2.5 and 10 ng/mL, respectively. The established HF-LPME method for the analysis of caffeine from aqueous sample can be used for the determination of biological, food and environmental samples.

• Analytical Science and Technology
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• v.22 no.4
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• pp.319-325
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• 2009

An effective and specific procedure for confirmation of neomycin, aminoglycoside antibiotic in honey was developed and validated. Honey was adjusted to pH 2 with 0.1M HCl and applied to weak cation-exchange SPE cartridge. Neomycin was eluted with basified methanol. Following separation by ion-pairing liquid chromatography, neomycin was analysed with positive electrospray ionization and MRM mode. Quantification was linear over the range of $5.0{\sim}250.0{\mu}g/kg$ ($r^2$ >0.9951). The precision (R.S.D.) and accuracy (as a bias) of quality control samples in honey ranged 11.5~18.7% and 10.9~20.9%, respectively. Established method can be applied to analysis of neomycin in honey.

• Analytical Science and Technology
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• v.21 no.5
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• pp.403-411
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• 2008

Dimethyldibutyltetradecylmalonamide (DMDBTDMA) extractant was used in a solvent extraction process for a radioactive liquid waste treatment. For the study of radiolysis phenomena, DMDBTDMA was synthesized and the degradation compounds (n-methylbutylamine, tetradecane, 1-tetradecanol) in the DMDBTDMA extractant, irradiated with $^{60}Co$ gamma ray, were identified and determined as radiolysis products by a Fourier transform infrared (FT-IR), gas chromatograph/mass spectrometer (GC/MS) analysis and GC/MS with selected ion monitoring (SIM) mode. Retention behavior of n-methylbutylamine, n-dodecane, tetradecane and 1-tetradecanol in the total ion chromatogram with the standard materials and n-dodecane as the internal standard (ISTD) were 2.35 min., 8.83 min., 10.68 min. and 12.75 min., respectively. In the case of tetradecane, there was a linear relationship between the concentration of the tetradecane and the absorbed dose of the ${\gamma}$-ray irradiated DMDBTDMA.

• Steel and Composite Structures
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• v.49 no.2
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• pp.143-159
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• 2023

Recently, the design of scaffolding systems has garnered considerable attention due to the increasing number of scaffold collapses. These incidents arise from the underestimation of imposed loads and the site-specific conditions that restrict the application of lateral restraints in scaffold assemblies. The present study is committed to augmenting the buckling resistance of vertical support members, obviating the need for supplementary lateral restraints. To achieve this objective, experimental and computational analyses were performed to assess the axial load buckling capacity of steel props, composed of two hollow steel pipes that slide into each other for a certain length. Three full-scale steel props with various geometric properties were tested to construct and validate the analytical models. The total unsupported length of the steel props is 6 m, while three pins were installed to tighten the outer and inner pipes in the distance they overlapped. Finite Element (FE) modeling is carried out for the three steel props, and the developed models were verified using the experimental results. Also, theoretical analysis is utilized to verify the FE analysis. Using the FE-verified models, a parametric study is conducted to evaluate the effect of different inserted pipe lengths on the steel props' axial load capacity and lateral displacement. Based on the results, the typical failure mode for the studied steel props is global elastic buckling. Also, the prop's elastic buckling strength is sensitive to the inserted length of the smaller pipe. A threshold of minimum inserted length is one-third of the total length, after which the buckling strength increases. The present study offers a prop with enhanced buckling resistance and introduces an equation for calculating an equivalent effective length factor (k), which can be seamlessly incorporated into Euler's buckling equation, thereby facilitating the determination of the buckling capacity of the enhanced props and providing a pragmatic engineering solution.

• Analytical Science and Technology
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• v.29 no.2
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• pp.94-103
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• 2016

An analytical method was developed to determine the amount of spinetoram (spinetoram J and spinetoram L) in livestock samples. The spinetoram was extracted with acetonitrile and purified through a primary secondary amine (PSA) sorbent. The spinetoram residues were then quantified and confirmed using a liquid chromatography–tandem mass spectrometer (LC-MS/MS) in the positive ion mode using multiple reactions monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005-0.5 mg/kg) into a blank extract with r² > 0.994. The limits of detection and quantification were 0.002 and 0.01 mg/kg, respectively. The recovery results of spinetram ranged between 81.9-106.4% at different concentration levels (LOQ, 10LOQ, 50LOQ, n=5) with relative standard deviations (RSDs) less than 10%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003). An interlaboratory study was conducted to validate the method. The proposed analytical method proved to be accurate, effective, and sensitive for spinetoram determination. The method will be used as an official analytical method in Korea.