An easily available, simultaneous identification/determination procedure for sildenafil, homosildenafil, tadalafil, vardenafil in adulterated health related foods was established by using a combination of three different analytical methods; thin layer chromatography(TLC), liquied chromatography-mass spectrometry (LC/MS) and high-performance liquied chromatography (HPLC)/photo-diode-array detector. The sample solution for TLC was applied to silica gel 60 $F_{254}$ plates with ethylacetate/acetonitrile/25%ammonia (90:10:5) as a developing solvent. Spots were located under UV radiation at 254 nm and dragendolfs reagent. Mass spectra of the compounds by LC/MS were investigated with electrospray ionization (ESI) interface, under positive ion mode. The HPLC analysis was performed on a column of capcell pack $C_{18}$ (UG120, 4.6${\times}$250mm I.D. 5 ${\mu}$m)with 0.1% sodium 1-hexansulfonate (in 0.1% phosphoric acid)/acetnitrile (73:27) as a mobile phase, and effluent was minitored with a photo-diode-applied to commercial foods, Sildenafil content was inthe range of 0.4mg/g~360.9 mg/g from 7 out of 35 samples. Homosildenafil content was in the range of 2.2 mg/g~336.0 mg/g from 7 out of 35 samples. Tadalafil content was 429.3 mg/g, 9.6 mg/500 mg from 2 out of 35 samples. The procedure described here is available for the screening of sildenafil, homosildenafil, tadalafil, vardenafil.
We have investigated Pi 2 pulsations which were observed both on ground magnetometer array and by satellites. On November 9th in 1994, Pi 2 pulsations appeared globally on the 190/210 magnetometer chain and Hermanus station when two satellites(EXOS-D and ETS-VI) were located near the magnetic meridian of the 210 array. The local time of measurements covers from morning(LT=8.47hr) to afternoon(LT=20.3hr) and the bandwidth of peak frequency is found relatively small. The signals of the electric field are highly coherent with ground-based observations with the out of phase oscillations. However, the magnetic field measurement on the ETS-VI in the outer magnetosphere(L=6.60) shows no signature of Pi 2 pulsations over the same time interval and the correlation with any of the ground-based stations is found to be very weak, even through both satellites and magnetometer chain are located close to each other in local time. We suggest that this event may be a direct evidence of Pi 2 pulsations as virtual resonant modes which are localized in the plasmasphere(Lee 1996). The results show that the cavity mode oscillations can occur in the inner magnetosphere with less spectral noise compared to the outer magnetospheric case.
Lee, Young-Jun;Choi, Jeong-Heui;Chung, Hyung Suk;Lee, Han Sol;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
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.
Oh, Mi Hyune;Lim, Moo Song;Chai, Jeung Young;Kim, Eun Jung;Cho, Joong Hoon;Lim, Chul Joo;Choi, Sun Ok
Journal of Food Hygiene and Safety
/
v.32
no.2
/
pp.89-95
/
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.
Proceedings of the Korean Radioactive Waste Society Conference
/
2005.11a
/
pp.321-331
/
2005
Recently. three-dimensional models have been used for aquatic dispersion of radioactive effluents in relation to nuclear power plant siting based on the Notice No. 2003-12 'Guideline for investigating and assessing hydrological and aquatic characteristics of nuclear facility site' of the Ministry of Science and Technology (MOST) in Korea. Several nuclear power plants have been under construction or planed. which are Shin-Korl Unit 1 and 2, Shin-Wolsong Unit 1 and 2, and Shln-Ulchin Unit 1 and 2. For assessing the aquatic dispersion of radionuclides released from the above nuclear power plants, it is necessary to know the coastal currents around sites which are affected by circulation of East Sea. In this study, a three dimensional hydrodynamic model for the circulation of the East Sea of Korea has been developed as the first Phase, which Is based on the RIAMOM. The model uses the primitive equation with hydrostatic approximation, and uses Arakawa-B grid system horizontally and Z-coordinate vertically. Model domain is $126.5^{\circ}E\;to\;142.5^{\circ}E$ of east longitude and $33^{\circ}N\;and\;52^{\circ}N$ of the north latitude. The space of the horizontal grid was $1/12^{\circ}$ to longitude and latitude direction and vortical level was divided to 20. This model uses Generalized Arakawa Scheme. Slant Advection, and Mode-Splitting Method. The input data were from JODC, KNFRDI, and ECMWF. The model ing results are in fairly good agreement with schematic patterns of the surface circulation in the East Sea The local current model and aquatic dispersion model of the coastal region will be developed as the second phase. The oceanic dispersion experiments will be also tarried out by using ARGO Drifter around a nuclear pelter plant site.
Design of the optical modulator composed of a three-waveguide coupler and CPW traveling-wave electrodes was carried out. Switching phenomena of three-waveguide couplers were analyzed by using the coupled mode theory, and the coupling-lengths of the devices were calculated by means of the FDM. CPW traveling-wave electrodes were analysed by the CMM and SOR simulation technique in order to find the conditions of phase-velocity and impedance matching. Traveling-wave modulators were fabricated on z-cut LiNbO$_3$ substrate. Ti was in-diffused in LiNbO$_3$ to make waveguides and Au electrodes were built on the waveguides by the electrolyte technique. The fabricated modulator chip was end-polished, pig-tailed and packaged in a brass mount with K-connector. The insertion loss and the switching voltage of the optical modulator were about 4㏈ and 19V, respectively. Network analyzer was used to obtain the S parameter and the corresponding RF response. From the measurement, parameters of the traveling-wave electrodes were extracted to be Z$_{c}$= 45 Ω, N$_{eff}$=2.20, and $\alpha$$_{0}$=0.055/cm√GHZ. The measured optical response R($\omega$) was compared with the theoretically estimated one, showing both responses agree well. The measurement results revealed that 3㏈ bandwidth turned out to be about 13 GHz.
Chung, Hyung Suk;Lee, Young Jun;Lee, Han Sol;Rahman, Md. Musfiqur;Kabir, Md. Humayun;Park, Byung-Jun;Kim, Jang-Eok;Shim, Jae-Han
Korean Journal of Environmental Agriculture
/
v.36
no.3
/
pp.201-210
/
2017
BACKGROUND: The current study was to monitor of 9 veterinary antibiotics (ceftiofur, clopidol, florfenicol, sulfamethazine, sulfamethoxazole, sulfathiazole, tetracycline, tiamulin, and tylosin) in manure using liquid chromatography-tandem mass spectrometry (LC-MS/MS) in positive and negative electrospray ionization mode. METHODS AND RESULTS: Sample preparation was carried out using Mcllvaine buffer and citrate salts to adjust the pH of the sample followed by purification with dispersive solid phase extraction (d-SPE). Separation of analytes during LC-MS/MS analysis was conducted using an Eclipse Plus $C_{18}$ column and the mobile phase was in gradient mode with, 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 of all tested antibiotics was good, with $R^2$ determination coefficients ${\geq}0.9920$. The limit of detection (LOD) and quantifications (LOQ) were $0.1-67.0{\mu}g/kg$ and $0.4-200.0{\mu}g/kg$, respectively. Analysis of 13 solid and liquid manure samples taken from the Republic of Korea revealed concentrations less than $0.7{\mu}g/kg$ for tiamulin, $1497.6{\mu}g/kg$ for sulfamethazine. CONCLUSION: To monitor 9 veterinary antibiotics from manure samples in 13 provincial areas throughout the Republic of Korea, an analytical method was developed. The developed method was fully validated and successfully applied for monitoring various veterinary antibiotics in manure samples.
The correlation and Empirical Orthogonal Function (EOF) analyses over the globe have been applied to intercompare lower-stratospheric (${\sim}$70hPa) temperature obtained from satellite data and two model reanalyses. The data is the19 years (1980-98) Microwave Sounding Unit (MSU) channel 4 (Ch4) brightness temperature, and the reanalyses are GCM (NCEP, 1980-97; GEOS, 1981-94) outputs. In MSU monthly climatological anomaly, the temperature substantially decreases by ${\sim}$21k in winter over southern polar regions, and its annual cycle over tropics is weak. In October the temperature and total ozone over the area south of Australia remarkably increase together. High correlations (r${\ge}$0.95) between MSU and reanalyses occur in most global areas, but they are lower (r${\sim}$O.75) over the 20-3ON latitudes, northern America and southern Andes mountains. The first mode of MSU and reanalyses for monthly-mean Ch4 temperature shows annual cycle, and the lower-stratospheric warming due to volcanic eruptions. The analyses near the Korean peninsula show that lower-stratospheric temperature, out of phase with that for troposphere, increases in winter and decreases in summer. In the first mode for anomaly over the tropical Pacific, MSU and reanalyses indicate lower-stratospheric warming due to volcanic eruptions. In the second mode MSU and GEOS present Quasi-Biennial Oscillation (QBO) while NCEP, El Ni${\tilde{n}}$o. Volcanic eruption and QBO have more impact on lower-stratospheric thermal state than El Ni${\tilde{n}}$o. The EOF over the tropical Atlantic is similar to that over the Pacific, except a negligible effect of El Ni${\tilde{n}}$o. This study suggests that intercomparison of satellite data with model reanalyses may estimate relative accuracy of both data.
Purpose: To perform the retrospective analysis of the sports injuries sustained by the college Taekwondo athletes in the respect of the injury patterns, mechanism of injury and clinical outcome Materials and Methods: This study is based on 47 out of 49 college Takwondo athletes, who had experienced the Takwondo related musculoskeletal injuries severe enough to visit the clinic for medical treatment. The mean age at the time of injury was 18.8 years and 39 were males and 8 females. The Taekwondo career was average 9.6 years and the injuries were sustained at average 6.7 years of their career. The injuries were analyzed by the detailed interview with thorough physical examination. Results: Forty-seven Taekwondo athletes in the study experienced average 1.8 injury/person (total 85 cases) with 26 persons of one time experience(55.3%), 11 persons of 2 times(23.4%),4 persons of 3 times (8.5%),5 persons of 4 times (10.6%) and 1 person of 5 times (2.2%). Injuries occurred during training in 50 cases (58.8%), while during match in 35 cases (41.2%). Injuries occurred during the attack phase of the match are 26 cases (31.7%) while 49 cases (57.6%) during the defense phase. As for the pattern of injury, fracture was the most common with 49 cases (57.6%), followed by ligament injury with 21 cases (24.7%). The upper extremity injuries were 32 cases (37.7%) while the lower extremity injuries were 44 cases (51.8%) Mode of medical treatment were operation in 15cases(17.7%), cast in 21 cases(24.7%), splint in 33 cases (38.8%), physical therapy in 15cases(17.7%) and acupuncture in 1 case(1.1%) Conclusion: Almost all the college Taekwondo athletes (96%) experienced sports injuries severe enough to receive medical treatments with the fracture being the most common injury pattern. The injuries occurred more commonly during the defense phase of the competition.
Sorafenib is a multikinase inhibitor and an oral anticancer drug approved for the treatment of patients with advanced renal cell carcinoma and those with unresectable hepatocellular carcinoma. The purpose of this study was to develop an efficient method of the determination of sorafenib in human plasma using tandem mass spectrometry coupled with liquid chromatography (LC/MS/MS) and validate the method by the guidelines of the Korean Food and Drug Administration (KFDA). Plasma samples ($100{\mu}l$) were added with chlorantraniliprole as an internal standard and then mixed with the 0.1% formic acid-containing extraction solution composed of isopropyl alcohol and ethyl acetate (1:4, v/v). After centrifugation, the supernatant was concentrated at $45^{\circ}C$ under negative pressure and centrifugal force. The residue was reconstituted with a mobile phase and injected into the HPLC instrument using a reverse phase Waters XTerra$^{TM}$ C18 column (particle size $3.5{\mu}m$). Liquid chromatography was carried out within the run time of 5 min using a mobile phase composed of buffer (0.1% formic acid and 10 mM ammonium formate), methanol, and acetonitrile (1:6:3, v/v/v). The analytes were monitored by tandem mass spectrometry in the multiple reaction monitoring method programmed to detect sorafenib at 'm/z 465.2 ${\rightarrow}$ 252.5' and chlorantraniliprole at 'm/z 484.4 ${\rightarrow}$ 286.2' with positive electrospray ionization mode ($ES^+$). The result showed the proper linearity ($r^2$ > 0.99) over the range of 2,000-5,000 ng/ml with good accuracy (90.7-103.9%) and precision (less than 10%). The newly developed method using LC/MS/MS was validated by the guideline of KFDA and identified as more sensitive compared to the previous methods.
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