• Analytical Science and Technology
• /
• v.20 no.4
• /
• pp.323-330
• /
• 2007

A simple and rapid HPLC method with fluorescence detection(FLD) for quantitation of penciclovir in human plasma using a monolithic column was developed and validated. Penciclovir and ganciclovir(internal standard, I.S.) were separated on a Chromolith column RP-18e ($4.6{\times}100mm$) with a mobile phase consisting of a mixture of (A) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (3/97, pH 2.5) and (B) methanol/50 mM sodium phosphate buffer containing 200 mg/L sodium dodecyl sulfate (50/50, pH 2.5) at a flow gradient of $1.6{\sim}4.0mL/min$. The retention times of penciclovir and internal standard were less than 4.0 min. Calibration curve was linear ($R^2=0.9994$) over a concentration range of $0.1{\sim}5{\mu}g/mL$. Intra-day precision, accuracy and inter-day precision were 1.36~8.55 %, 92.8~100.0 % and 0.93~5.62 %, respectively with a limit of quantitation at $0.1{\mu}g/mL$. The present HPLC-FLD method is sensitive, precise and accurate. The method described herein has been successfully used for the bioequivalence study of a famciclovir formulation product after oral administration to healthy Korean volunteers.

• KSCE Journal of Civil and Environmental Engineering Research
• /
• v.29 no.1B
• /
• pp.35-45
• /
• 2009

In this study, a laboratory experiment has been performed on a S-curved channel with two curved sections. In the experiments, effects of 3-D velocity structures on mixing characteristics of tracer material were investigated. As a result, it was clearly noticed that the primary flow travels taking the shortest course of the meandering channel and has a very ununiform distribution at the bends. The secondary cell which was developing at the first bend disappears at the crossover, and then, at the next bend, secondary cell is re-developing in the opposite direction. The experimental results show that mixing of tracer is significantly affected by the combined action of ununiform primary flow and secondary cell. The ununiform primary flow separates the tracer cloud in the longitudinal direction, and the secondary cell further separates the retarding tracer cloud mainly in the transverse direction. As a result, these complex flow structures cause separation and spreading of tracer cloud both in the longitudinal and in the transverse directions. The measured dimensionless transverse dispersion coefficients calculated using 2-D routing procedure ranges 0.012-0.875, and is generally proportional to width to depth ratio (W/h). The predicted values calculated by the theoretical equation overestimate slightly the measured transverse dispersion coefficients.

• The Journal of the Convergence on Culture Technology
• /
• v.9 no.6
• /
• pp.867-873
• /
• 2023

In this study, for the purpose of standardized quality control of a cold medicine, we simultaneous analyzed four main chemical components of a cold medicine: acetaminophen, caffeine, methyl paraben, and propyl paraben. The sample was subjected to quantitative analysis using high performance liquid chromatography (HPLC), after pretreatment of four components. The experiment was carried out by using Isocratic elution at wavelength of 270nm. Acetonitrile and water (H₂O) were used as a mobile phase at a flow rate of 1.0mL/min in a commercial C18 reversed-phase column. A volume of 10uL cold medicine were injected into the column with column oven temperature at 35℃. As a result of the experiment, the values of Resolution were 4.983, 1.596, 5.519, and 1.678 respectively-well over Rs >1.5, which indicates that the separation of four components were efficient. In addition, value of symmetry factor of the components was 1.056, 1.069, 1.032, and 1.133 respectively, to show its symmetrical stability. The calibration curve of all four components exhibits good linearity with R² >0.9995 to 0.9999. Furthermore, the limit of detection(LOD) were between 0.0118 to 1.5973 mg/mL, while the limit of quantification (LOQ) were between 0.0353 to 4.7919 ㎍/mL with the recovery rate of 79.6% ~ 120.5%. The results of this study showed an efficient quality evaluation of a simultaneous analysis method for cold medicine components.

• Korean Journal of Ichthyology
• /
• v.19 no.4
• /
• pp.350-359
• /
• 2007

The egg development and morphological change of larvae and juveniles of the starry flounder, Platichthys stellatus were observed in laboratory. Fertilized eggs of the species, 1.09~1.19 mm (mean $1.13{\pm}0.03mm$, n=50) in diameter, were floating, colorless, transparent in shape and lacked in oil globules. The eggs hatched out 121 hours after fertilization at water temperature $8.2{\sim}11.2^{\circ}C$. The size of the hatched larvae were 2.58~2.89 mm (mean $2.67{\pm}0.09mm$) in total length, their mouth and anus were not open yet and myotome number was 14+27=41. Melanophore and xanthophore appeared on the notochord and digestive organ and the margin of membrane fin, on the yolk sac and eyes were lacking in pigment cells. 5 days after hatching the larvae attained 4.30~4.97 mm (mean$4.74{\pm}0.21mm$) in TL, and their mouth and anus were open. 10 days after hatching the larvae transformed to postlarval stage and they were 4.67~5.75 mm in TL (mean $5.30{\pm}0.31mm$), and absorbing the yolk completely. Feeding activity increased as the mouth became larger. At 23 days, the larvae attained 6.69~8.82 mm in TL (mean $7.85{\pm}0.75mm$), and the right eye was started moving to the left side of the head. At 52 days, the juveniles attained 10.99~17.06 mm in TL (mean $13.50{\pm}1.67mm$). The right eye was moved completely onto the left side. All of the fins had completed set of the fin rays (D. 64~67: A. 45~51: P. 11: V. 6: C. 19).

• Korean Journal of Agricultural Science
• /
• v.2 no.2
• /
• pp.331-339
• /
• 1975

This experiment was carried out to obtain some imformations about the ecological variations of the heading time of the newly breeded Indica x Japonica varieties/pedigrees according to the seasonal changes of the seeding date. day length and temperature. The results obtained are summarized as follows; 1) At all varieties. days to heading showed a straight reduction according as the seeding time was delayed. 2) At the group of Japonica varieties. the days to heading of early maturing varieties were much shortened and that of medium or late maturing varieties were little or not shortened under high temperature condition but at the group of Indica ${\times}$ Japonica va rieties/pedigrees. days to heading were significantly elongated under high temerature condition. 3) At the group of Japonica varieties. the effect of the short day condition on the days to heading was significantly high at the medium and the late maturing varieties than at the early maturing varieties. however. the short day effect on the reduction of days to heading was not related with the earlyness of each varieties at the group of Indica ${\times}$ Japonica varieties/pedigrees. 4) Days to heading of all varieties under the high temperature condition were longer than that under the ordinary culture. On the other hand, the days to heading of Japonica varieties under the short day treatment were shorter than the days to heading of ordinary culture but at the group of Indica x Japonica varieties/pedigrees. the days to heading under the short day treatment were longer than ordinary culture. 5) At both varieties groups. the days to heading at each seeding time were significantly correlated with days to heading at ordinary cultivation. fl) At the group of Japonica varieties. relatively high correlation(p=0.1) was recognized between the days to heading by delay of seeding time, but at the group of Indica ${\times}$ Japonicava rieties/pedigrees, correlation between the ordinary heading date and the shortening rate of days to heading was very low.

• Journal of Life Science
• /
• v.22 no.11
• /
• pp.1456-1462
• /
• 2012

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.

• Journal of the Korean Society of Food Science and Nutrition
• /
• v.46 no.10
• /
• pp.1186-1194
• /
• 2017

Recently, many people have demanded reliable nutritional data even for minor-components. On the other hand, an analytical method for the analyses of vitamin $B_5$ and $B_6$ is lacking. Therefore, this study attempted to validate with accuracy and precision the analysis of vitamin $B_5$ and $B_6$ using a high-performance liquid chromatography (HPLC) method. The vitamin $B_5$ and $B_6$ contents were analyzed using an Agilent 1260 series HPLC system. YMC-Pack ODS-AM ($250{\times}4.6mm$ I.D.) and YMC-Pack Pro RS $C_{18}$ ($250{\times}4.6mm$ I.D.) columns were used for the analyses of vitamin $B_5$ and $B_6$, respectively. In the case of vitamin $B_5$, the flow rate was set to 1.0 mL/min by isocratic elution using the 50 mM $KH_2PO_4$ solution (pH 3.5)/acetonitrile (ACN) (95:5, v/v) with monitoring at 200 nm using HPLC/DAD, whereas the flow rate for vitamin $B_6$ was set to 1.0 mL/min of flow rate by isocratic elution using a 20 mM $CH_3CO_2Na$ solution (pH 3.6)/ACN (97:3, v/v) with monitoring by excitation at 290 nm and emission at 396 nm using HPLC/FLD. The column temperature was set to $30^{\circ}C$. The injection volume was $20{\mu}L$ for each experiment. The specificity of the accuracy and precision for vitamin $B_5$ and $B_6$ were also validated by HPLC. The results showed high linearity in the calibration curve for vitamin $B_5$ ($R^2=0.9998^{{\ast}{\ast}}$), the limit of detection (LOD) and limit of quantitation (LOQ) were 0.4 mg/L and 1.3 mg/L, respectively, In contrast, for the calibration curve of vitamin $B_6$, which showed high linearity ($R^2=0.9999^{{\ast}{\ast}}$), the LOD and LOQ were 0.006 mg/L and 0.02 mg/L, respectively.

• Korean Journal of Food Science and Technology
• /
• v.44 no.6
• /
• pp.686-691
• /
• 2012

The objective of this research is to present method development and validation for the simultaneous determination of lutein and zeaxanthin using ultra performance liquid chromatography (UPLC). Also, rapid quantification was performed on six green leafy vegetables (Allium tuberosum, Aster scaber, Hemerocallis fulva, Pimpinella brachycarpa, Sedum sarmentosum and Spinacia oleracea) that are commonly consumed in Korea. Separation and quantification were successfully achieved with a Waters Acquity BEH C18 ($50{\times}2.1mm$, $1.7{\mu}m$) column by 85% methanol within 5 min. Two compounds showed good linearity ($r^2$ > 0.9968) in $1-150{\mu}g/mL$. Limit of detection (LOD) and quantification (LOQ) for lutein and zeaxanthin were 1.7 and 5.1 g/mL and 2.1 and 6.3 g/mL, respectively. The RSD for intra- and inter-day precision of each compound was less than 10.69%. The recovery of each compound was in the range of 91.75-105.13%. Aster scaber and Spinacia oleracea contained significantly higher amounts of lutein ($4.06{\pm}0.24$ and $3.97{\pm}0.10mg$/100 g of fresh weight), respectively.

• KOREAN JOURNAL OF CROP SCIENCE
• /
• v.3
• /
• pp.41-48
• /
• 1965

This study was aimed at knowing the magnitude of year variation in rice heading dates under the different seasonal cultures, and to estimate the heading date in advance. Using six rice varieties such as Kwansan, Suwon＃82, Suwon ＃144, Norin＃17, Yukoo＃132 and Paltal, the early, ordinary and late seasonal cultures had been carried out at Paddy Crop Division, Crop Experiment Station at Suwon for the six-year period 1959 to 1964. In addition the data of the standard rice cultures at the Provincial Offices of Rural Development for the 12-year period 1953 to 1954, were analyzed for the purpose of clarifying a relationship between variation of rice heading dates and some of meteorological data related to the locations and years. The results of this study are as follows: 1. Year variation of rice heading dates was as high as 14 to 21 days in the early seasonal culture and 7 to 14 days in the ordinary seasonal culture, while as low as one to seven days in the late seasonal culture which was the lowest among three cultures. The magnitude of variation depended greatly on variety, cultural season and location. 2. It was found out that there was a close negative correlation between the accumulated average air temperature for 40 days from 31 days after seeding and number of days to heading in the early seasonal culture. Accordingly, it was considered possible to predict the rice heading date through calculation of the accumulated average air temperature for the above period and then the linear regression(Y=a+bx). On the other hand, an estimation of the heading date in the late seasonal culture requires for the further studies. In the ordinary seasonal culture, no significant correlation between the accumulated average air temperature and number of days to heading was obtained in the six-year experiments conducted at Suwon. There was a varietal difference in relationship between the accumulated average air temperature for 70 days from seeding and number of days to heading in the standard cultures at the provincial offices of rural development. Some of varieties showed a significant correlation between two factors while the others didn't show any significant correlation. However, there was no regional difference in this relationship.

• Korean Journal of Environmental Agriculture
• /
• v.30 no.3
• /
• pp.288-294
• /
• 2011

BACKGROUND: Methylmercury is analyzed by HPLC-ICP/MS because of the simplicity for sample preparation and interference. However, most of the pre-treatment methods for methylmercury need a further pH adjustment of the extracted solution and removal of organic matter for HPLC. The purpose of this study was to establish a rapid and accurate analytical method for determination of methylmercury in fish by using HPLC-ICP/MS. METHOD AND RESULTS: We conducted an experiment for pre-treatment and instrument conditions and analytical method verification. Pre-treatment condition was established with aqueous 1% L-cysteine HCl and heated at $60^{\circ}C$ in microwave for 20 min. Methylmercury in $50{\mu}L$ of filtered extract was separated by a C18 column and aqueous 0.1% L-cysteine HCl + 0.1% L-cysteine mobile phase at $25^{\circ}C$. The presence of cysteine in mobile phase and sample solution was essential to eliminate adsorption, peak tailing and memory effect problems. Correlation coefficient($r^2$) for the linearity was 0.9998. The limits of detection and quantitation for this method were 0.15 and $0.45{\mu}g/kg$ respectively. CONCLUSION: Result for analytical method verification, accuracy and repeatability of the analytes were in good agreement with the certified reference materials values of methylmercury at a 95% confidence level. The advantage of the established method is that the extracted solution can be directly injected into the HPLC column without additional processes and the memory effect of mercury in the ICP-MS can be eliminated.