• Mass Spectrometry Letters
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• v.10 no.3
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• pp.88-92
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• 2019

A sensitive analytical method of rhodanthpyrone A in rat plasma was developed using a liquid chromatography-tandem mass spectrometry (LC-MS/MS). Rhodanthpyrone A and rhodanthpyrone B (internal standard) in rat plasma were extracted by a liquid-liquid extraction method with ethyl acetate. This extraction method gave results in high and reproducible extraction recovery in the range of 73.75-79.90% with no interfering peaks around the peak elution time of rhodanthpyrone A and B. The standard calibration curves for rhodanthpyrone A ranged from 0.5 to 2000 ng/mL were linear with $r^2$ > 0.994 and the inter- and intra-day accuracy and precision and the stability were within acceptance criteria. Using this validated analytical method, pharmacokinetics of rhodanthpyrone A following intravenous and oral administration of rhodanthpyrone A at doses of 2 mg/kg and 30 mg/kg, respectively, were investigated. Rhodanthpyrone A in rat plasma showed multi-exponential elimination pattern with high clearance and volume of distribution values. The absolute oral bioavailability of this compound was calculated as 3.7%. Collectively, the newly developed sensitive LC-MS/MS analytical method of rhodanthpyrone A could be successfully applied to investigate the pharmacokinetic properties of this compound and would be useful for the further studies on the efficacy, toxicity, and biopharmaceutics of rhodanthpyrone A.

• Korean Journal of Veterinary Service
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• v.42 no.3
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• pp.127-133
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• 2019

The purpose of this study was to investigate the contamination level of representative mycotoxins that have adverse effects on livestock by using LC-MS/MS method and to utilize the results as basic data for the establishment of quality control system for feed, and to provide information on production and storage. A total of nine mycotoxins, including aflatoxin $B_1$, aflatoxin $B_2$, aflatoxin $G_1$, aflatoxin $G_2$, ochratoxin A, fumonisin $B_1$, fumonisin $B_2$, deoxynivalenol (DON), zearalenone (ZEN) were simultaneously analyzed in LC-MS/MS under ESI positive mode. Fumonisin $B_1$ and fumonisin $B_2$ were detected from 3 cases of 75 forage produced in Incheon area, the detection rate was 4.0%. The detection concentration was 0.01~0.02 mg/kg, which was lower than the domestic recommended limit. Fumonisins were detected in a slightly different manner from the results of mycotoxin studies reported in Korea, which is attributed to the high temperature and dry summer weather of the year. The result of LC-MS/MS method performance of 9 mycotoxins, the recovery of DON was quite low as $41.53{\pm}3.91%$ that is not suitable for simultaneous analysis. This is probably due to that the extract solution used in this study was not suitable for the extraction of DON, along with the characteristics of a very dry forage. For the study of mycotoxins in Incheon area forage for the first time, further investigation is needed for the safe supply of livestock products.

• Journal of Korean Society of Environmental Engineers
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• v.32 no.4
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• pp.349-356
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• 2010

Ion chromatography (IC) coupled with conductivity detector (CD) is a common system for the determination of perchlorate in water samples. Although the IC method with CD has been widely used for the determination of trace level perchlorate ion in water, sensitivity decreases dramatically as the complexity of the matrices increases. Here we proposed the application of ion chromatography coupled with mass spectrometry (IC-MS/MS) to significantly improve selectivity of perchlorate. The mean recovery of the method was 104.4 ${\pm}$ 5.7% and the relative standard deviation (RSD%) was 1.9 ${\pm}$ 1.3%. The alculated method detection limit (MDL) was 0.0207 ${\pm}$ 0.0099 ${\mu}g/L$. The concentrations of perchlorate were minimum <0.1 ${\mu}g/L$ and maximum 18.3 ${\mu}g/L$ in source water (Namhan, Bukhan and Han River). Hongreung showed higher concentrations ($1^{st}$-14.3 ${\mu}g/L$, $2^{st}$-18.3 ${\mu}g/L$) than the other places. And the concentrations of perchlorate were 0.18~0.34 ${\mu}g/L$ in the samples taken from the six water treatment plants and six intake stations in Seoul.

• Analytical Science and Technology
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• v.21 no.3
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• pp.191-200
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• 2008

Pharmaceuticals and personal care products (PPCPs) are emerging contaminants in aquatic environmental samples. Therefore, it required rapidly and certainly analytical method for pharmaceuticals which are existed in environment. In this study, Liquid chromatography/tandem mass spectrometry (LC-MS/MS) with electrospray ionization (ESI) was used to measure the concentrations of 7 pharmaceuticals (quinoxaline-2-carboxylic acid, acetylsalicylic acid, diclofenac-Na, naproxen, ibuprofen, mefenamic acid, talniflumate) from environmental water or aquatic samples simultaneously. Effective sample clean-up by solid-phase extraction (SPE) prior to LC-MS/MS analysis is necessary. For further purification, Mixed Cation eXchange (MCX) and Hydrophilic-Lipophilic Balance (HLB) solid-phase extraction (SPE) cartridges were used to eliminate the remaining interferences. LODs (Limits of Detection) and MDLs (Method Detection Limits) for the spiked sample in fresh water were in the range of 0.05~1.50 pg/mL and 0.17~4.90 pg/mL, respectively. The absolute recovery in the concentration of 1.0 ng/mL were between 81.9 and 116.3%. The acidic pharmaceuticals were detected in concentrations of 0.018~16.925 ng/mL in aquatic environmental samples.

• KIPS Transactions on Computer and Communication Systems
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• v.4 no.3
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• pp.97-104
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• 2015

This paper will feature designs for security vulnerability based on MS-SQL Database and OLE connectivity by checking the MS-SQL database password policy, the user account password access attempts, a user without password, and password does not be changed for a period of time. This paper uses the MS-SQL database and C++ linkage in order to use the OLE DB function. The design module should judge presence or absence of security vulnerability by checking database password policy, the user account password access attempts, a user without password, password does not be changed for a period of time. The MS-SQL database password associated with a feature, judging from the many features allows you to check for security vulnerability. This paper strengthen the security of the MS-SQL database by taking the advantage of the proposed ability.

• Korean Journal of Food Science and Technology
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• v.41 no.4
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• pp.458-463
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• 2009

To establish and validate a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for the rapid and accurate quantitation of diarrhetic shellfish poisoning (DSP) toxins, we compared the results from different mobile phases and columns used for their analysis and collision energies for MS/MS experiments. Clear peaks of okadaic acid (OA) and dinophysistoxin-1 (DTX1) were obtained by using a mobile phase comprising aqueous acetonitrile containing 2 mM ammonium formate and 50 mM formic acid. The collision energies were optimized to facilitate the most sensitive detection for each toxin, namely, OA, DTX1, pectenotoxin-2 (PTX2), or yessotoxin (YTX). Further, the maximum ion response was obtained at a collision energy of 48 V for OA and DTX1. We compared the analytical performance of $C_8$ and $C_{18}$ columns. A wide range of toxins namely, OA, DTX1, PTX2, and YTX, except DTX3, were detected by both the columns. Although DTX3 was only detected by the $C_8$ column, we found that the $C_{18}$ column was also suitable for the quantitation of OA and DTX1 the toxins responsible for inducing diarrhea. The limit of detection of OA and DTX1 by the established LC-MS/MS conditions was 1 ng/g, and the limit of quantitation of the toxins under the same conditions was 3 ng/g. The process efficiencies were 91-118% for oysters (Crassostrea gigas) and 96-117% for mussels (Mytilus galloprovincialis) further, we observed no significant effect of matrix during the ionization process in LC-MS/MS. The comparison between mouse bioassay (MBA) and LC-MS/MS yielded varying results because low concentrations of OA and DTX1 were detected by LC-MS/MS in some shellfish samples, which provided positive results on MBA for DSP. The analysis time required by MBA for DSP analysis can be reduced by LC-MS/MS.

• Korean Journal of Medicinal Crop Science
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• v.14 no.4
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• pp.225-228
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• 2006

To acquire the normal regeneration of plantlets, we investigated combinations and concentrations of plant growth regulations for optimal conditions of adventitious root formation. Based on the previous study, we performed callus and shoot induction. When induced shoot was transferred into a rooting medium containing plant hormones, it wilted and died. Thus, the shoot proliferated on 1/2 MS medium for 10 days and was then treated with MS medium supplemented with 3.0 mg/L NAA for 3 days. Adventitious root formations were observed after shoot planlets were transferred to 1/3 MS medium. The concentrations of salt and sucrose were gradually reduced in MS medium and the rooted plantlets were transferred for acclimatization into a mixture of peatmoos : perlite (3 : 2).

• YAKHAK HOEJI
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• v.55 no.1
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• pp.56-63
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• 2011

Fabry disease (FD) is an X-linked inborn error of glycoshpingolipid metabolism resulting from mutation in the enzyme ${\alpha}$-galactosidase A gene. The disease is an X-linked lipid storage disorder and the lack of ${\alpha}$-Gal A causes an intracellular accumulation of glycosphingolipids, mainly globotriaosylceramide (Gb-3). Measurement of Gb-3 in plasma has clinical importance for monitoring after enzyme replacement therapy for confirmed FD patients. Using electrospray ionization MS/MS we had developed, a simple, rapid, and highly sensitive analytical method for Gb-3 in plasma was used for the purpose of screening FD among high risk groups in Korean population. To date, no comprehensive results for FD screening have been performed and reported in Korea. We screened 1,100 outpatients from 13 hospitals (including clinics) to assess the incidence of FD among patients in high risk groups. For patients with borderline level amount of Gb-3, we repeated Gb-3 or performing complementary or confirmative assay with ${\alpha}$-Gal A activity and DNA mutaion analysis for confirmation diagnosis. Of 1,100 we diagnosed 3 FD with 2 classical type and 1 carrier (0.27%).

• Korean Journal of Pharmacognosy
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• v.47 no.1
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• pp.92-101
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• 2016

In this study, an ultra-performance liquid chromatography-electrospray ionization-mass spectrometry (UPLC-ESI-MS/MS) method was established for simultaneous determination of the 25 marker components, including chlorogenic acid, gallic acid, oxypaeoniflorin, homogentisic acid, methyl gallate, caffeic acid, 3,4-dihydroxybenzaldehyde, paeoniflorin, albiflorin, liquiritin, nodakenin, ferulic acid, ginsenoside Rg1, liquiritigenin, coumarin, cinnamic acid, benzoylpaeoniflorin, ginsenoside Rb1, cinnamaldehyde, paeonol, glycyrrhizin, 6-gingerol, evodiamine, rutecarpine, and spicatoside A in traditional Korean formula, Onkyung-tang. All analytes were separated on a Waters Acquity UPLC BEH $C_{18}$ analytical column ($2.1{\times}100mm$, $1.7{\mu}m$) at $45^{\circ}C$ using a mobile phase of 0.1% (v/v) formic acid in water and acetonitrile with gradient elution. The MS analysis was carried out using a Waters ACQUITY TQD LC-MS/MS coupled with an electrospray ionization (ESI) source in the positive and negative modes. The flow rate and injection volume were 0.3 mL/min and $2.0{\mu}L$, respectively. The correlation coefficient of all analytes in the test ranges was greater than 0.98. The limits of detection and quantification values of the 25 marker compounds were in the ranges 0.03-19.43 and 0.09-58.29 ng/mL, respectively. As a result, methyl gallate, 3,4-dihydroxybenzaldehyde, evodiamine, and rutecarpine were not detected in this sample and the concentrations of the 21 compounds except for the above 4 compounds were $33.09-3,496.32{\mu}g/g$ in Onkyung-tang decoction. Among these compounds, paeonol was detected at the highest amount as a $3,496.32{\mu}g/g$.

• 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.