• Bulletin of the Korean Chemical Society
• /
• v.34 no.6
• /
• pp.1684-1688
• /
• 2013

A rapid and sensitive method for determining usnic acid of Lethariella cladonioides in rat was established using high performance liquid chromatography (HPLC) quadrupole time-of-flight (QTOF) tandem mass (MS/MS). Rat plasma was pretreated by mixture of acetonitrile and chloroform to precipitate plasma proteins. Chromatographic separation was achieved on a column ($50{\times}2.1$ mm, $5{\mu}m$) with a mobile phase consisting of water (containing $5{\times}10^{-3}$ M ammonium formate, pH was adjusted to 3.0 with formic acid) and acetonitrile (20:80, v/v) at a flow rate of 0.3 mL/min. A tandem mass spectrometric detection with an electrospray ionization (ESI) interface was conducted via collision induced dissociation (CID) under negative ionization mode. The MS/MS transitions monitored were m/z 343.0448 ${\rightarrow}$ m/z 313.2017 for usnic acid and m/z 153.1024 ${\rightarrow}$ m/z 136.2136 for protocatechuic acid (internal standard). The linear range was calculated to be 2.0-160.0 ng/mL with a detection limit of 3.0 pg/mL. The inter- and intra-day accuracy and precision were within ${\pm}7.0%$. Pharmacokinetic study showed that the apartment of usnic acid in vivo confirmed to be a two compartment open model. The method was fully valid and will probably be an alternative for pharmacokinetic study of usnic acid.

• Journal of the Korean Society for Railway
• /
• v.20 no.1
• /
• pp.85-98
• /
• 2017

In general, under the repetitive dynamic load generated by rail cars running on the track, subgrade soil experiences changes of stress conditions such as deviatoric stress (${\sigma}_d$) and bulk stress (${\theta}$). Due to the repetitive change of deviatoric stress (${\sigma}_d$) with number of loadings, the resilient modulus ($M_R$) can be obtained by using the measured resilient strain (${\varepsilon}_r$) after a sufficient number of loadings. At present, no plausible and unified test method has been proposed to obtain the resilient modulus of railway track subgrade soil. In this study, a possible test method for obtaining the resilient modulus ($M_R$) of railway track subgrade soil is proposed; this test, by utilizing repetitive triaxial compression testing, can consider all the important parameters, such as the confining stress, deviatoric stress, and number of loadings. By adapting and using the proposed test method to obtain $M_R$, $M_R$ values for compacted track subgrade soil can be successfully determined using soil obtained in three field sites of railway track construction with changing water content range from OMC. In addition, shear modulus (G) ~ shear strain (${\gamma}$) relation data were also obtained using a mid-size RC test. A correlation analysis was performed using the obtained G and $M_R$ values while considering the strain levels and modes of strain direction.

• Korean Journal of Food Science and Technology
• /
• v.47 no.1
• /
• pp.1-5
• /
• 2015

This study aimed to simultaneously determine various carotenoids from different colored paprika using an ultra performance liquid chromatograph (UPLC) equipped with a HSS T3 column. Analysis was performed at 450 nm using gradient conditions with acetonitrile/methanol/methylene chloride (65/25/10) and distilled water. We improved the peak resolution and performed carotenoid analysis within 30 min. We qualitatively analyzed 11 carotenoids (neoxanthin, capsorubin, violaxanthin, capsanthin, zeaxanthin, lutein, ${\alpha}$-cryptoxanthin, ${\beta}$-cryptoxanthin, lycopene, ${\alpha}$-carotene, and ${\beta}$-carotene). For the validation of UPLC methods, we validated the precision and accuracy of capsanthin. Capsanthin showed good linearity ($R^2$=0.9998) in the concentration range of $1-200{\mu}g/mL$ with 2.4 and $7.2{\mu}g/mL$ of limit of detection (LOD) and limit of quantification (LOQ), respectively. The relative standard deviation (RSD) for intra- and inter-day precision was less than 3.83%. Recovery was in the range of 91.86-99.87%. We quantitatively analyzed carotenoid contents from 8 different colored paprika (red, orange, yellow, and green). The most abundant carotenoids were capsanthin in red paprika, and zeaxanthin in orange, yellow, and green paprika.

• Korean Journal of Environmental Agriculture
• /
• v.35 no.3
• /
• pp.166-174
• /
• 2016

BACKGROUND: The current study developed a monitoring method of 6 veterinary antibiotics (amoxicillin, ampicillin, enrofloxacin, tetracycline, chlortetracycline, oxytetracycline) in agricultural soils using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive electrospray ionization mode.METHODS AND RESULTS: Sample preparation was carried out using acidic acetonitrile and citrate salts followed by purification with dispersive solid phase extraction (d-SPE). Separation on Eclipse Plus C₁₈ column was conducted in gradient of the mobile phase, 0.1% formic acid and 5 mM ammonium formate in methanol (A) and 0.1% formic acid and 5 mM ammonium formate in distilled water (B). The linearity of the matrix-matched calibrations expressed as the coefficient of determination was good with R²≥0.9900. The limit of quantifications (LOQs) ranged from 0.5 to 10 μg/kg for all analytes. Analysis of 51 agricultural soil samples taken in the Republic of Korea revealed concentrations less than 1.9 μg/kg for enrofloxacin, 75.5 μg/kg for chlortetracycline.CONCLUSION: The method was successfully applied to monitor 6 veterinary antibiotics from 51 field incurred agricultural soil samples in 17 provincial areas throughout the Republic of Korea. The developed method was simple, easy, and versatile and can be used for monitoring various veterinary antibiotics in soil.

• Analytical Science and Technology
• /
• v.28 no.6
• /
• pp.460-466
• /
• 2015

An isotope dilution liquid chromatography tandem mass spectrometry was developed as a primary method for the quantitative analysis of cholesterol in infant formula. Cholesterol-d₄ was used as an internal standard and spiked into the infant formula sample. In order to release cholesterol out of cholesteryl ester, which is cholesterol bound to fatty acids in infant formula, saponification was carried out. Saponification conditions were optimized with heating temperature, reaction time and the concentration of KOH. The optimum conditions were as follows; heating temperature was 70 ℃, reaction time was 180 min and the concentration of KOH was 0.8 mL of 8 M KOH for about 0.1 g infant formula sample. Extraction of cholesterol out of sample solution was carried out with hexane uisng liquid-liquid extraction. Chromatographic analysis was carried out using Phenomenex Kinetex C₁₈ column. Mobile phase was 0.1% acetic acid in methanol/water (v/v, 99/1) and flow rate was 0.3 mL/min. Cholesterol and cholesterol-d₄ were monitored at mass transfer m/z 369/259 and 373/263 respectively. Reproducibility of the method was evaluated to be 0.23% of the measurement result. The expanded uncertainty of the measurement result of cholesterol in infant formula was approximately 1.9% at a 95% confidence level. NIST standard reference material having certified values of cholesterol in infant formula, was analyzed in order to verify this method. The ID-LC/MS/MS results were well agreed with the certified values of NIST SRM within the uncertainty.

• Journal of the Korean Society of Clothing and Textiles
• /
• v.33 no.6
• /
• pp.980-989
• /
• 2009

Amur cork tree was extracted in methanol with the purpose of investigating the most effective extraction procedure for detecting the chromophore using the GC-MS analysis. Different procedures of waterbath and hotplate extractions were carried out and five different GC-MS instrument parameters including the operating temperatures in the GC capillary column and the MSD scan range were tested for their efficiencies. Berberine was determined by the detection of dihydroberberine at 15.0 min r.t. Hotplate was a better device for extracting amur cork tree than waterbath shaker either with or without presoaking in the room temperature. Water was not an adequate extraction medium for the berberine detection. The most effective GC-MS parameter was Method 4; the initial temperature at $50^{\circ}C$ followed by the temperature increase of $23^{\circ}C$/min until $210^{\circ}C$, then increase of $30^{\circ}C$/min until the final temperature reach at $305^{\circ}C$, then hold for 14 minutes to maintain the total run time 24.12 minutes. The MSD scan range for Method 4 was $35\sim400$m/z.

• Journal of the Korea Concrete Institute
• /
• v.22 no.3
• /
• pp.409-417
• /
• 2010

This paper discusses a series of experiments including material improvement in order to ensure quality of grouting for the post-tensioned structure. In prestressed concrete, grouting refers to the construction procedure of filling empty space of duct enclosing with strands using cementitious material, To date, adequate quality control of the grouting has not been established in Korea because the relationship between the grouting and durability of post-tensioned structure is not well-recognized. The Korean standard does not consider the important material characteristic, wick effect, which is caused by strands in the ducts and current standard testing method unlikely quantify reasonable material segregation. As a result, the grout material, which meets the current material standards, may exhibit excessive bleeding water or shrinkage during construction. In this study, international codes and standards related to grouting were surveyed. The ratio of constituents and novel admixtures were suggested to meet equivalently with these standards. Performance of this enhanced grout was compared to common domestic grout using the international standard testing method. A series of mock-up specimens considering geometry of PC beam was constructed and grout flow pattern was observed as the grout was injected. It was observed that the grouting performance was highly influenced by material properties and filling characteristic can be varied depending on geometry of ducts.

• Journal of Aquaculture
• /
• v.9 no.3
• /
• pp.239-245
• /
• 1996

As one of the red tide control method, montmorillonite was used to eliminate the causative organisms in Korea and Japan. We assayed the loess to replace the montmorillonite because it distribute in large quantity and nearby the red tide occurrence in South Coast of Korea. By using the mixture of loess and coal ashes, we examined the decreasing level of nutrients such as ammonia and phosphate, the elimination of causative organisms as a chlorophyll a content, and the harmful effect on aquaculture orgarnisms in cage culture farms. Half of the ammonium and phosphate was adsorbed by the loess particles, but only $25\%$ of ammonium was adsorbed by the coal ashes particles. In water column test, the particles of loess and coal ashes were settled down by $80\%$ in 20 minutes, the red tide organisms was eliminated by $80\%$ after 2 hours in 1,000 ppm of loess suspension, but the organisms were eliminated only $30\%$ by the same concentration of coal ashes. The harmful test of fishes and invertbrates, we observed any other negative effects of test animals than a tint deceleration in yellowtail.

• Korean Journal of Environmental Biology
• /
• v.24 no.3
• /
• pp.240-247
• /
• 2006

The dynamic of zooplankton community and its relationship with dissolved oxygen were studied at the Soho area of Gamak Bay from 22 August to 15 September in summer. We found that zooplankton were in low abundance or absent from bottom waters when oxygen concentrations were <3 mg $L^{-1}$. The relationship between summer low-oxygen in bottom-layer and zooplankton community structure was discussed at vertical abundance in Soho area of Gamak Bay. To examine effects of bottom-layer low-oxygen on abundance and vertical distributions in the stratified Soho area, zooplankton was surveyed near-surface, within the near-bottom in the study area under a range of near-bottom dissolved oxygen conditions. There were vertical variation in total zooplankton abundance in the study area (ANOVA, P<0.05). Overall abundance of zooplankton: copepod nauplii, Oithona sp. and tintinnids were lower throughout the water column when bottom-layer DO was low (${\leq}3mg\;L^{-1}$). In this context it was postulated that zooplankton distribution in the Soho area of Gamak Bay might be controlled by dissolved oxygen condition.

• Journal of the Korean Society of Clothing and Textiles
• /
• v.31 no.12
• /
• pp.1653-1661
• /
• 2007

The research aimed to establish the standard extraction procedure for examining brazilin, the major chromophoric substance of Sappanwood, using GC-MS with the ultimate goal of identifying the sappanwood dye in severely faded archaeological textiles. The amount of brazilin represented by the GC abundance was the largest when acetone was used as the extraction medium, followed by methanol. Shaking plate operated at room temperature was more effective than the waterbath shaker which was operated at $30^{\circ}C$. In both cases, the extraction method which incorporated one hour pre-soaking before the 12 hours of actual extraction resulted in a larger amount of brazilin detection than the extraction procedure without the one hour pre-soaking. In case of water extraction, pH 5 resulted in the most effective pH level for the extraction of brazilin, The best GC-MS parameter for detecting brazilin was to set the column temperature initially at $50^{\circ}C$. gradually increase to $210^{\circ}C$ at a $23^{\circ}C/min$ rate, finally increase to $305^{\circ}C$ at $30^{\circ}C/min$ rate, and hold for 14 minutes, and the MSD scan range at $75{\sim}400m/z$.