• 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.

• Analytical Science and Technology
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• v.29 no.2
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• pp.57-64
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• 2016

Many phthalic acid esters (PAEs), including DMP, DEP, DBP, BBP, and DEHP, as well as DEHA are widely used as plasticizers in plastics. An analytical method was developed and used to analyze these compounds at 41 industrial facilities. The coefficient of determination (R²) for each constructed curve was higher than 0.98. The method detection limit (MDL) values were 0.4–0.7 μg/L for PAEs and 0.6 μg/L for DEHA. In addition, the recovery rate was shown to be 77.0–92.3%, while the relative standard deviation was shown to be in the range of 5.8-10.5%. DMP (n = 3), DEP (n = 2), DBP (n = 2), BBP (n = 2), and DEHA (n = 3) were detected in the range of 2.2-11.1% in the influent. DEHP was a predominant compound and was detected at > MDL in both the influent (n = 16, 35.6%) and the effluent (n = 4, 10.0%) at a high removal efficiency (92–100%). The highest levels of residue in industrial wastewater influent were 137.4 μg/L of DEHP at plastic products manufacturing facility, 12.5 μg/L of DEHA at a chemical manufacturing facility, and 14.0 μg/L of DEP at an electronics facility. The highest concentration of effluent was 12.5 μg/L of DEHP at a chemical manufacturing facility, which indicated that the effluent was below the allowable concentration (800 μg/L). Therefore, the levels of PAEs and DEHA that are discharged into nearby streams could not influence the health of the ecosystem.

• Analytical Science and Technology
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• v.26 no.4
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• pp.287-297
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• 2013

The optimization of analytical method for the thermal desorption of seven VOCs (volatile organic compounds) by TD-GC/MS (thermal desorption-gas chromatograph-mass spectrometer) with solid phase sorbent tube, and comparative analysis for the determination of VOCs plotted by standard sorbent tubes prepared using both gas phase and liquid phase materials were investigated. The result of paired t-test showed that a liquid phase standard sorbent tube method was in agreement with a gas phase standard sorbent tube method for six species of VOCs including benzene, toluene, ethylbenzene, o-, m-, and p-xylene except for styrene at the significance level (${\alpha}=0.01$), while the 15.6% of difference in response factor between both of gas phase and liquid phase standard plotting for the determination of styrene showed that both methods were significantly different at the significance level. Therefore, the liquid phase standard plotting method was employed to reduce erroneous data for the determination of styrene including BTEX. Under the optimized analytical method by liquid phase standard sorbent tube, recovery was between $100{\pm}5%$ for 7 species of VOCs, reproducibility ranged from 0.3 to 7.7%, and method detection limit (MDL) ranged from $0.01{\mu}g/m^3$ for o-xylene to $0.27{\mu}g/m^3$ for toluene. The optimized standard method was applied to determine VOCs VOCs from indoor air of of dormitory, one bedroom apartment, and a new car.

• Journal of the Speleological Society of Korea
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• no.63
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• pp.1-8
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• 2004

The non-magnetic materials with non-conductive showing high structure dispersity were developed on the base of natural quartz and lava-scoria which was collected from Je-ju island in Korea, and treated by methane-chemical technology those were obtained novel properties of magnetization through the analyzing. Depending on the processing conditions and subsequent applications the materials produced by strong methane-chemical reaction (MCR) in alcohol solution showed concurrently magnetic, dielectric and electrical properties. The obtained magnetic-electrical powders classified by aggregate complex of their features as segnetomagnetics, containing a dielectric material as a carrying nucleus, particularly the quartz on that surface one or more layers of different compounds were synthesized having thickness up to 10～50 nm and showing magnetic, electrical and other properties. It was confirmed in magnetizing process that powders of quartz and lava-scoria produced by MCR were better oil adsorbent as of oleophilic and floating matter on water surface although their specific gravities are comparably more than 1 in quartz or less than unity, as that of water, in lava-scoira. Therefore, it will be Possible and very useful to remove low density and light gravity oil spillage in difficult recovery from sea and inland water contamination spread on water surface, by marine accident and ship sinking accident occurring frequently in recent years, by way of magnetic adsorbent conveyer system in continuous, if it could be built up the mass Production system of water-floating magnetizable oleophilic adsorbent materials with use of iow cost and good Qualify lava-scoria spread on volcano district in Je-ju island. And, there will also be urgent advent of necessity with strong possibility to develop useful applications of various magnetic functional materials include oleophilic adsorbent for removal of sea oil-contaminants and maritime pollutants, and other kinds of various utilities in industrial applications and practical uses of novel functional materials in the fields of environments and health care applications with in deep expectation.

• Progress in Medical Physics
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• v.21 no.2
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• pp.201-208
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• 2010

Recently, along with technology development of endoscopic equipment, a stent has been developed for the convenience of operation, shortening of recovery times, and reduction of patient's pain. To this end, optimal factors are simulated for the stent structure and mechanical reaction and verified using finite element analysis. In order to compare to present commercialized product such as Zilver (Cook, Bloomington, Indiana, USA) and S.M.A.R.T (Cordis, Bridgewater Towsnhip, New Jersey, USA), mechanical impact factors were determined through Taguchi factor analysis, and flexibility and expandability of all the products including ours were tested using finite element analysis. Also, important factors were sought that fulfill the optimal condition using central composition method of response surface analysis, and optimal design were carried out based on the important factors. From the centra composition method of Response surface analysis, it is found that importat factors for flexibility is stent thickness (T) and unit area (W) and those for expandability is stent thickness (T). In results, important factors for optimum condition are 0.17 mm for stent thickness (T) and $0.09\;mm^2$ for unit area (W). Determined and verified by finite element analysis in out research institute, a stent was manufactured and tested with the results of better flexibility and expandability in optimal condition compared to other products. Recently, As Finite element analysis stent mechanical property assessment for research much proceed. But time and reduce expenses research rarely stent of optimum coditions. In this research, Important factor as mechanical impact factor stent Taguchi factor analysis arrangement to find flexibility with expansibility as Finite element analysis. Also, Using to Center composition method of Response surface method appropriate optimized condition searching for important factor, these considering had design optimized. Production stent time and reduce expenses was able to do the more coincide with optimum conditions. These kind of things as application plan industry of stent development period of time and reduce expenses etc. be of help to many economic development.

• Analytical Science and Technology
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• v.25 no.4
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• pp.257-264
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• 2012

Penicillins belong to the ${\beta}$-lactam class of antibiotics, and are frequently used in human and veterinary medicine. Despite the positive effects of these drugs, improper use of penicillins poses a potential health risk to consumers. This study has been undertaken to determinate multi-residues of penicillins, including amoxicillin, ampicillin, oxacillin, bezylpenicillin, cloxacillin, dicloxacillin, and nafcillin, using liquid chromatographic tandem mass spectrometer (LC-MS/MS). The developed method was validated for specificity, precision, recovery, and linearity in livestock and marine products. The analytes were extracted with 80% acetonitrile and clean-up by a single reversed-phase solid-phase extraction step. Six penicillins presented recoveries higher than 76% with the exception of Amoxicillin. Relative standard deviations (RSDs) were not more than 10%. The method was applied to 225 real samples. Benzylpenicillin was detected in 12 livestock products and 7 marine products. Amoxicillin, ampicillin, cloxacilllin, dicloxacillin, nafcillin and oxacillin were not detected. The detected levels were 0.001~0.009 mg/kg in livestock products excluding eggs and milk. In marine products, the detected levels were under 0.03 mg/kg. They were under the MRL levels. As monitoring results, it is identified to be safe but it is considered that safety management of antibiotics should continue by monitoring.

• Analytical Science and Technology
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• v.25 no.1
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• pp.76-82
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• 2012

The determination and confirmation of dutasteride in human serum was performed by a liquid chromatography-electrospray ionization tandem mass spectrometry (LC-ESI/MS/MS). Beclomethasone as an internal standard (I.S.) was added to the serum and the mixed sample was pretreated by liquid-liquid extraction (LLE) with methyl tert-butyl ether (MTBE). The mass transitions of dutasteride and I.S. monitored in multiple reaction monitoring (MRM) were m/z 529.6${\rightarrow}$461.5 and m/z 409.3${\rightarrow}$391.2, respectively, and the retention times were 6.45 and 5.46 min, respectively. The calibration curve was linear in the concentration range of 0.5~30.0 ng/mL ($R^2$= 0.9999) and the limit of quantitation (LOQ) was found to be 0.5 ng/mL. The recovery of dutasteride was shown to be 66~72%. The intra-day assay precision and accuracy were in the range 3.5~5.5% and 85.7~89.9%, respectively, and the interday assay precision and accuracy were in the range 4.2~5.8% and 90.8~95.8%, respectively.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.33 no.5
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• pp.431-438
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• 2000

To clarify the annual reproductive cycle in a rockfish, Sebastes schlegeli, monthly changes in gonadosomatic index (GSI), hepatosomatic index (HSI) and histological feature of gonads and plasma levels of sex steroid hormones ($estradiol-l7{\beta},\;17{\alpha},\;20{\beta}-dihydroxy-4-pregnen-3-one,\;testosterone\;and\;11-ketotestosterone$) were investigated. The annual reproductive cycle in females could be divided into 5 periods as follows: 1) recovery period (June to September): serum level of $estradiol-l7{\beta}$ increased gradually; 2) vitellogenesis period (Septemer to february) : vitellogenic oocytes were obsewed, GSI sustained high value, and serum level of $estradiol-l7{\beta}$ increased; 3) gestation period (February-April): developing larva showed in the ovary, and serum levels of $17{\alpha},\;20{\beta}-dihydroxy-4-pregnen-3-one$ and testosterone increased; 4) partrition period (April to May) : larva were delivered, and value of GSI and serum levels of hormones decreased rapidly; 5) resting period (May to June) : value of GSI and serum levels of $estradiol-l7{\beta}$ and testosterone remained low. The annual reproductive cycle in males could be divided into 6 periods; 1) early maturation period (April to June): value of GSI and serum levels of hormones incresed gradually, cyst of spermatogonia incresed in number, and a small number of cyst of spermatocyte was observed; 2) mid-maturation perid (June to September); value of GSI and serum levels of hormones increased, and germ cells in many cysts were undergoing active sperrnatogenesis; 3) late maturation period (September to November) : value of GSI and serum levels of hormones remained high and spermatozoa were released into the lumina of the seminal lobules; 3) spermatozoa dischaging period (Nobember to December) : the lumina of the seminal lobules were enlarged and filled with mature spermatozoa; 4) degeneration period (December to Februauy)i value of GSI decresed and cyst of spermatocyte were decresed in number; 5) resting period (December to April) : no histological changes of testes were observed, and value of GSI and serum levels of hormones remained low. In November, the lumina of the seminal lobules were filled with mature spermatozoa and sperm masses were present in the ovarian cavity. Thus, copulation in this species occurred in November and December.

• Journal of Life Science
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• v.24 no.3
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• pp.252-259
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• 2014

The leaves of Peatasites japonicus are a traditional oriental medicine with diverse biological activities. A simple and specific analytical method for the quantitative determination of bakkenolide B constituents from methanolic extract of the leaves of P. japonicus was developed. Bakkenolide B was isolated from the leaves of P. japonicus, and its structure was elucidated based on 1D, 2D NMR, and GC-MS spectral data. A liquid chromatographic method was developed to evaluate the quality of P. japonicus through determination of major active compound, bakkenolide B. The wavelengths at 254 and 215 nm were chosen to determine bakkenolide B. The recovery of the method was in the range of 98.6 to 103.1%, and bakkenolide B showed good linearity ($r^2$=0.999) within test ranges. The developed method was applied to the determination of bakkenolide B in the plant part and seasonal changes. The results showed that the content of bakkenolide B in the leaf was higher than in the petiole and rhizome. In this study, a simple, rapid, and reliable high-performance liquid chromatography method was used to determine the percentage and composition of bakkenolide B in P. japonicus procured from different Petasites species plants in South Korea. The method can be employed in routine quantitative analysis and quality control of different products in the market.

• Food Science and Preservation
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• v.20 no.4
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• pp.451-458
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• 2013

The purpose of this research is to distinguish the quantitative determination of phytochemicals in various agricultural products and to optimize an HPLC method for the determination of lycopene, lutein, ${\alpha}$-carotene, ${\beta}$-carotene, and cryptoxanthin. Among the different conditions studied, the most suitable ones for our samples were the extraction with hexane/acetone/ethanol (50:25:25, v/v/v), dissolution of the dry extract in tetrahydrofuran/acetonitrile/methanol (15:30:55, v/v/v), injection on a $C_{18}$ column with methanol/acetonitrile (90:10, v/v) + triethylamine $9{\mu}M$ as mobile phase, and ${\lambda}_{detection}$=475 nm. The mean percent recovery for the HPLC method were $120.7{\pm}4.1%$ (lycopene), $89.2{\pm}3.5%$ (lutein), $91.2{\pm}2.9%$ (${\alpha}$-carotene), $99.1{\pm}4.4%$ (${\beta}$-carotene), and $100.0{\pm}5.3%$ (cryptoxanthin). The contents of lutein in the agricultural products were spinach, kiwi, tomato, blueberry, melon, respectively. However, the lycopene contents were the highest in the Black tomato ($56.66{\pm}7.48mg/kg$) and Jangseong tomato ($50.28{\pm}5.42mg/kg$). The concentration of ${\beta}$-carotene in all of the agricultural products ranged from 0.07 mg/kg to 65.03 mg/kg. The quercetin content of the agricultural products increased in the order of blueberry (986.57~1,054.06 mg/100 g), kiwi (44.96~55.09 mg/100 g), hallabong (31.92~35.60 mg/100 g), and tomato (26.38~34.94 mg/100 g). The highest kaempferol content was found in the blueberry (47.79~76.15 mg/100 g) with results in all of the tested samples varying between 6.54~48.11 mg/100 g. The total polyphenol contents of the various agricultural products increased in the blueberry (213.60~229.96 mg/100 g), spinach (112.50~141.67 mg/100 g) and kiwi (46.49~70.44 mg/100 g). The total flavonoid content was the highest in both blueberry and spinach. Vitamin C content was detected in kiwi > hallabong > tomato > blueberry, respectively. The total anthocyanin contents (TAC) was detected in the Damyang blueberry and the imported blueberry.