• Analytical Science and Technology
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• v.30 no.1
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• pp.10-19
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• 2017

Anabolic steroids have similar structures to testosterone, both of which promote the growth of muscle mass and increase strength. However, the side effects of anabolic steroid use may lead to heart attacks or strokes. Additionally, the excessive use of steroids inhibits the production of the sex hormones in the body via a negative feedback loop, which results in testicular atrophy in males and amenorrhea in females. Currently, the method of choice used to test for the presence of anabolic steroids is GC-MS. However, GC-MS methods require chemical derivatization of the steroid sample to ensure compatibility with the analytical method; therefore, analysis of many different samples is difficult and time consuming. Unlike GC-MS, the liquid chromatography-quadrupole-time of flight mass spectrometry (LC-Q-TOF-MS) method is suitable for many samples. Twenty-two different anabolic steroids were analyzed by LC-Q-TOF-MS with various collision energies (CE). Accurate mass spectral data were obtained using a Q-TOF-MS equipped with an electro-spray ionization source and operated in the positive MS/MS mode for several classes of steroids that are often the targets of testing. Based on the collected data, fragmentation pathways were carefully elucidated. The high selectivity and sensitivity of the LC-Q-TOF-MS instrument combined with these fragmentation pathways offers a new approach for the rapid and accurate screening of anabolic steroids. The obtained data from the 22 different anabolic steroids will be shared with the scientific community in order to establish a library to aid in the screening of illegal anabolic steroids.

• Analytical Science and Technology
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• v.29 no.5
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• pp.242-247
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• 2016

This research aims to set up and validate methods of analyzing the methanol in wet wipes and verifies the analysis methods that applied to the wet wipes. We used Headspace (HS) Gas Chromatography (GC) - Flame Ionization Detector (FID) to the establish analysis method of methanol in wet wipes and optimized heating temperature, heating time, GC conditions with column. The result indicated that 3 mL of sample in 20 mL headspace vial can be equilibrated efficiently in headspace sampler at 70 ℃ for 10 min and sample was measured by GC with spli injection mode(10:1). The results show that linearity from 1 to 100 ppm was over R2 0.9995, precision was RSD 1.83 % and accuracy(recovery rate) was 105.44 (±1.05 %) on water matrix and wet wipes matrix removed non-woven fabric. Also, monitoring results of total 20 cosmetics on the market, from 0.00017 to 0.00156 % of methanol was detected from wet wipes.

• YAKHAK HOEJI
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• v.51 no.2
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• pp.96-102
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• 2007

Measurement of globotriaosylceramide (Gb3, ceramide trihexoside) in urine has clinical importance for monitoring after enzyme replacement therapy in Fabry disease patients. The disease is an X-linked lipid storage disorder that results from a deficiency of the enzyme ${\alpha}$-galactosidase A (${\alpha}$-Gal A). The lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly Gb3. A simple, rapid, and highly sensitive analytical method for Gb3 in urine was developed without labor-extensive pre-treatment by electrospray ionization MS/MS (ESI-MS/MS). Only simple 5-fold dilution of urine is necessary for the extraction and isolation of Gb3 in urine. Gb3 in diluted urine was dissolved in dioxane containing C17:0 Gb3 as an internal standard. After centrifugation it was directly injected and analyzed through guard column by in combination with multiple reaction monitoring mode of ESI-MS/MS. Eight isoforms of Gb3 were completely resolved from urine matrix. C24:0 Gb3 occupied 50% of total Gb3 as a major component in urine. Linear relationship for Gb3 isoforms was found in the range of 0.005${\sim}$5.0 ${\mu}$g/ml. The limit of detection (S/N=5) was 0.005 ${\mu}$g/ml and limit of quantification was 0.05 ${\mu}$g/ml for C24:0 Gb3 with acceptable precision and accuracy. Correlation coefficient of calibration curves for 8 Gb3 isoforms ranged from 0.9598 to 0.9975. This method could be useful for rapid and sensitive 1st line Fabry disease screening, monitoring and/or diagnostic tool for Fabry disease.

• Journal of Food Hygiene and Safety
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• v.32 no.2
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• pp.89-95
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• 2017

A rapid, sensitive analytical method for glucuronolactone in beverages was developed and validated using hydrophilic interaction liquid chromatography coupled to electrospray ionization tandem mass spectrometry (HILIC-ESI-MS/MS). To determine the optimum analytical conditions for glucuronolactone, three different kinds of HILIC columns and two mobile phases with different pH values were examined. An amide-bonded stationary phase with a pH 9 acetonitrile-rich mobile phase was the best condition in terms of column retention, ESI-MS/MS response area, and signal-to-noise ratio. After extraction, glucuronolactone was separated through the HILIC amide column and detected by negative ESI-MS/MS in selected reaction monitoring (SRM) mode. Nine energy drinks sold in Korea were spiked with glucuronolactone at a concentration of 5 ng/mL; the Monster $Energy^{TM}$ sample showed the smallest peak area and its signal-to-noise ratio was used for method validation. Good linearity was obtained in the concentration range from 20 to 1500 ng/mL with a correlation coefficient > 0.998. The developed method had a limit of detection (LOD) of 6 ng/mL and a limit of quantitation (LOQ) of 20 ng/mL. The recovery of this method at concentration of 20, 100, 500, and 1000 ng/mL was 96.3%-99.2% with relative standard deviations (RSD) of 1.6%-14.0%. A reproducibility precision assessment at concentration of 100 and 500 ng/mL was carried out among three laboratories. The recovery of that evaluation was 95.1%-102.3% with RSD of 2.7%-7.0%. An analysis of variance indicated that there was no difference between the recovery results of the three laboratories at the 5% significance level. The validated method is applicable to inspecting beverages adulterated with glucuronolactone in Korea.

• Analytical Science and Technology
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• v.22 no.4
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• pp.326-335
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• 2009

A specific analytical method able to identify and quantify traces of six glucocorticoids residues in eggs were developed. The extraction and clean-up parameters for simultaneous analysis were evaluated and HPLC and spectrometric conditions were also established. For determination of glucocorticoids, 5 g of egg was transferred into a test tube, adjusted pH 5.2 with acetate buffer and was $\beta$-glucuronidase/arylsulfatase from Helix pomatia added. The mixture was centrifuged and supernatant was extracted twice with 20 mL n-hexane. The extraction was performed with HLB cartridge using methanol, followed by clean-up with silica cartridge using methanol/ethyl acetate (4/6, v/v). The analytes were determined by HPLC/ESI-MS/MS operating in the negative ion mode. Validation studies with fortified egg samples for established method were performed. The result of method validation gave good efficiency, linearity, accuracy and precision. The correlation coefficients ($r^2$) of the calibration curves appeared to be higher than 0.99 in egg, indicating excellent linearity. LOD was ranged 0.09 to $0.17{\mu}g/kg$, and recoveries for most compounds were in the range of 55.7-69.8%. This method can be used to determine ${\mu}g/kg$ levels of glucocorticoids in eggs.

• Preventive Nutrition and Food Science
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• v.10 no.1
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• pp.95-102
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• 2005

The term pharmacognosy as applied to a constituent scientific discipline of Korean Medical Food (KMF) has been in use for nearly several years, and it refers to studies on the pharmacological properties of natural products foods. During the last half of the 20th century, pharmacognosy for KMF evolved from being a descriptive botanical subject to one having a more chemical and biological focus. At the beginning of the 21st century, teaching pharmacognosy for KMF teaching in academic culinary arts and natural healing institutions has been given new relevance as a result of the explosive growth in the use of herbal foods (health foods) in modern KMF practice. In turn, pharmacognosy for KMF research areas are continuing to expand, and now include aspects of cellular and molecular biology in relation to natural products, ethnobotany and phytotherapy, in addition to the more traditional analytical method development and phytochemistry. Examples are provided in this review of promising bioactive compounds obtained in two multidisciplinary natural product KMF development and discovery projects, aimed at the elucidation of new plant-derived cancer chemotherapeutic agents and novel cancer chemopreventives, respectively. The systematic study of KMF offers pharmacognosy groups an attractive new area of research, ranging from investigating the biologically active principles of KMF and their mode of action and potential active substance interactions, to sanitary and quality control, and involvement in clinical trials.

• Journal of Korean Society of Steel Construction
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• v.10 no.3 s.36
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• pp.407-421
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• 1998

The purpose of this paper is to provide and verify an analytical method, based on the spline finite strip method, which can be used to investigate the buckling mode and stress of thin-walled steel sections. Geometric imperfection and initial stress of plates and plate assemblies, which are resulted from various preloadings and may cause prebuckling deformations before buckling, are included in the analysis. Material nonlinearity and residual stress are also considered. It can be applied to sections with simple or non-simple boundary conditions and arbitrary loading. The method has been applied to investigate the buckling behavior of plates and plate assemblies which are subjected to compression with initial imperfections and residual stresses.

• Journal of Korea Society of Industrial Information Systems
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• v.16 no.5
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• pp.21-30
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• 2011

In this paper, we propose a real-time service based on retransmission slot in low rate WPAN. In the proposed scheme, during the communication period of the beacon-enabled mode in LR-WPAN standard, a special GTSs is dynamically assigned for retransmission of the packet that fails during a real-time service such as voice. This provides a time diversity in the severe channel error environments to support the required QoS. Analytical results show that this scheme achieves a much higher throughput and better transmission success rate per GTS slot than conventional schemes such as a common reserved scheme in LR WPAN.

• Structural Engineering and Mechanics
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• v.33 no.2
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• pp.239-255
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• 2009

In the companion paper, a simple but effective analysis procedure termed an Improved Modal Pushover Analysis (IMPA) is proposed to estimate the seismic capacities of multi-span continuous bridge structures on the basis of the modal pushover analysis, which considers all the dynamic modes of a structure. In contrast to previous studies, the IMPA maintains the simplicity of the capacity-demand curve method and gives a better estimation of the maximum dynamic response in a bridge structure. Nevertheless, to verify its applicability, additional parametric studies for multi-span continuous bridges with large differences in the length of adjacent piers are required. This paper, accordingly, concentrates on a parametric study to review the efficiency and limitation in the application of IMPA to bridge structures through a correlation study between various analytical models including the equivalent single-degree-of-freedom method (ESDOF) and modal pushover analysis (MPA) that are usually used in the seismic design of bridge structures. Based on the obtained numerical results, this paper offers practical guidance and/or limitations when using IMPA to predict the seismic response of a bridge effectively.

• Structural Engineering and Mechanics
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• v.11 no.3
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• pp.237-258
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• 2001

Structural identification via modal analysis in structural mechanics is gaining popularity in recent years, despite conceptual difficulties connected with its use. This paper is devoted to illustrate both the capabilities and the indeterminacy characterizing structural identification problems even in quite simple instances, as well as the cautions that should be accordingly adopted. In particular, we discuss an application of an identification technique of variational type, based on the measurement of eigenfrequencies and mode shapes, to a steel frame with friction joints under various assembling conditions. Experience has suggested, so as to restrict the indeterminacy frequently affecting identification issues, having resort to all the a priori acknowledged information on the system, to the symmetry and presence of structural elements with equal stiffness, to mention one example, and mindfully selecting the parameters to be identified. In addition, considering that the identification techniques have a local character and correspond to the updating of a preliminary model of the structure, it is important that the analytical model on the first attempt should be adequately accurate. Secondly, it has proved determinant to cross the results of the dynamic identification with tests of other typology, for instance, static tests, so as to fully understand the structural behavior and avoid the indeterminacy due to the nonuniqueness of the inverse problem.