• Korean Journal of Pharmacognosy
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• v.38 no.2 s.149
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• pp.192-196
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• 2007

A rapid and practical HPLC assay was developed for quantitative analysis of saponins in Platycodi Radix. Seven saponin components in Platycodi Radix, i.e., deapioplatycoside E, platycoside E, deapioplatycodin D$_3$, platycodin D$_3$, polygalacin D$_2$, platycodin D$_2$ and platycodin D were successfully resolved on C18 column and detected by ELSD. Standard curves were linear over the concentration range 1 ${\sim}$2,000 ${\mu}$g/ml (r$^2$>0.992). Intra- and inter-day coefficients for variation of seven saponin components were < 10% and limit of quantification of them were around 0.7${\sim}$1.5 ${\mu}$g/ml, respectively. Using this method, contents of seven saponins in various plant materials under different cultivating conditions were estimated.

• YAKHAK HOEJI
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• v.52 no.1
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• pp.12-19
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• 2008

The organic acids (formic acid, acetic acid and propionic acid), phenol and benzopyrene in wood vinegar were determine by HPLC. An $Atlantis^{TM}dC_{18}$ column with a acetonitrile: 0.1% phosphoric acid (5: 95, organic acids), acetonitrile: water (10 : 90, phenol), 100% acetonitrile (benzopyrene) as a mobile phase was used. Retention time of acetic acid, formic acid, propionic acid, phenol and benzopyrene was 4.77, 3.73, 9.08, 30.97 and 6.10 min, respectively. The calibration curves of organic acids, phenol, benzopyrene were linear over the concentration range of $30{\sim}500,\;60{\sim}1000$, and $3{\sim}50\;{\mu}g/ml$ with correlation coefficient of above 0.999. The limit of detection (LOD) and limit of quantitation (LOQ) of acetic acid, formic acid, propionic acid, phenol, and benzopyrene was 1.71 and 5.19, 1.11 and 3.35, 4.87 and 14.74, 6.45 and 19.55, 0.08 and $0.24\;{\mu}g/ml$, respectively. The coefficients of variation for intra- and inter-day assay were $0.21{\sim}4.14$ and $0.07{\sim}1.19%$, respectively and the precision was $95{\sim}115%$. From this study, we suggest that HPLC is suitable method for the determination of organics in wood vinegar and could be applied to quality control of wood vinegar.

• YAKHAK HOEJI
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• v.49 no.3
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• pp.212-216
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• 2005

A rapid, sensitive and selective electrospray tandem mass spectrometric (ESI-LC/MS/MS) method for the quantitation of gliquidone in human plasma was developed. A bioavailability study of gliquidone tablet (30 mg gliquidone, Boehringer Ingelheim Korea Co.) was performed using the validated ESI-LC/MS/MS method. The dose of 30 mg of gliquidone (1 tablet) was orally administered to 9 healthy Korean subjects. After administration, blood was taken at 0.5, 1, 1.5, 2, 2.5, 3, 3.5, 4, 5, 7, 9, 12, 24, and 33 hour. The validation data were as follows; the standard curve was linear ($r^2$=0.999) over the concentration range of $10\~1000 ng/ml$. The coefficient of variation for intra- and inter-day assay were $8.30\~18.86$, and $2.19\~12.92\%$, respectively. The lower limit of quantification for gliquidone was 10 ng/ml. The pharmacokinetic parameters obtained were as follows; $AUC_t$ was 3861.17$\pm$1328.61 ng-hr/ml, $C_{max}$ was 831.02$\pm$227.99 ng/ml, $T_{max}$ was $2.94{\pm}0.77 hr,\;K_e$, was 0.19$\pm$0.06 1/hr, and $t_{l/2}$ was 4.47$\pm$3.52 hr. Based on the validated analytical method and pharmacokinetic parameters, a standard guideline of the bioavailability test of gliquidone dosage forms was prepared successfully and could be used for the bioequivalence test of gliquidone preparation.

• YAKHAK HOEJI
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• v.49 no.3
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• pp.225-229
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• 2005

A rapid, sensitive and selective tandem mass spectrometric method (LC-MS/MS) for the quantitation of nicorandil in human plasma was developed. A bioavailability study of Sigmat tablet (5 mg nicorandil, Choongwae Co.) was per-formed using the validated LC-MS/MS method. The dose of 5 fig of nicorandil (1 tablet) was orally administered to 9 healthy Korean subjects. After administration, blood was taken at 0.25, 0.5, 1, 2, 3, 4, 5, 6, 9, 12, and 24 hour. The validation data were as follows; the standard curve was linear ($r^2$=0.999) over the concentration range of $0.5\~200.0 ng/ml$. The coefficient of variation for intra- and inter-day assay were $3.55\~7.44$, and $2.17\~9.102\%$, respectively. The lower limit of quantification for nicorandil was 0.5 ng/ml. The pharmacokinetic parameters obtained were as follows; $AUC_t$ was 145.9$\pm$83.0 ng-hr/ml, Cmax was 83.8$\pm$32.2 ng/ml, $C_{max}$ was 0.42$\pm$0.13 hr, $K_e$ was 0.56$\pm$0.23 l/hr, and $t_{l/2}$ was 1.42$\pm$0.52 hr. Based on the validated analytical method and pharmacokinetic parameters, a standard guideline of the bioavailability test of nicorandil dos-age forms was prepared successfully and could be used for the bioequivalence test of nicorandil preparation.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.55 no.6
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• pp.917-926
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• 2022

The green turtle Chelonia mydas has been designated as an endangered species globally due to its reduced population. Although C. mydas is not known to reproduce on the shores of the Korean peninsula, it has been listed as a protected marine species in South Korea. This study describes the first successful captive breeding of C. mydas in a commercial aquarium in South Korea and provides information on the early growth patterns of C. mydas hatched and reared in indoor facilities. C. mydas YS-B003 laid a total of 594 eggs in ten nesting events in the period December 2016-June 2017. Of these, 115 fertilized eggs from six events hatched successfully. The size of the newly hatched turtles differed significantly among nesting events. The hatchlings from the 8^th and 9^th nesting events were relatively smaller than those from the 3^rd and 5^th events. The rate of growth initially varied across the different events, but from the 1,000^th day, the inter-group variation disappeared. The present study provides useful information for future captive breeding of sea turtles in indoor facilities, which would contribute to the protection of these endangered sea turtle species.

• Bulletin of the Korean Chemical Society
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• v.32 no.8
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• pp.2648-2656
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• 2011

A simple HPLC-DAD method was developed and validated to determine B group vitamin content (thiamine, riboflavin, nicotinamide, pantothenic acid, pyridoxine and folic acid) in supplemented food samples, i.e., infant formula, cereal, low-calorie food, a multi-vitamin pill and a vitamin drink. In this study, the most significant advantages were simultaneous determination of the six B group vitamins in various food matrices and a small number of sample treatment steps that required only an organic solvent, acetonitrile. Moreover, this method prevents reduction of column durability, because the mobile phase does not contain ion-pairing reagents. Analytes were separated on a Develosil RPAQUEOUS $C_{30}$ (4.6 mm ${\times}$ 250 mm, 5 ${\mu}M$ particle size) column with a gradient elution of acetonitrile and 20 mM phosphate buffer (pH 3.0) at a flow rate between 0.8 and 1.0 mL/min. Detection was performed at 275 nm, except for that of pantothenic acid (205 nm). The calibration curves for all six vitamins showed good linearity with correlation coefficients ($r^2$) higher than 0.995. The developed method was validated with respect to linearity, intra- and inter-day accuracy and precision, limit of quantification (LOQ), recovery and stability. The method showed good precision and accuracy, with intra- and inter-assay coefficients of variation less than 15% at all concentrations. The recovery was carried out according to the standard addition procedure, with yields ranging from 89.8 to 104.4%. This method was successfully applied to the determination of vitamin B groups in supplemented food products.

• YAKHAK HOEJI
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• v.51 no.2
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• pp.133-139
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• 2007

A simple and sensitive HPLC-MS method for quantitation of 10${\alpha}$-methoxy-9,10-dihydrolysergol (MDL), the main metabolite of nicergoline, in human plasma was developed and the bioavailability parameters of MDL was assessed in Korean healthy male volunteers. Clomipramine was used as an internal standard. MDL and internal standard in plasma sample were extracted using ethyl acetate. A centrifuged upper layer was then evaporated and reconstituted with mobile phase of 10 mM ammonium acetate-acetonitrile (10 : 90, v/v). The reconstituted samples were injected into a Zorbax SB-C8 column (2.1${\times}$150 mm,5 ${\mu}$m) at a flow-rate of 0.3 ml/min. Using MS with selected ion monitoring (SIM) mode, MDL and clomipramine were detected without severe interference from human plasma matrix. MDL produced a protonated molecular ion ([M+H]$^+$) at m/z 287. Internal standard produced a protonated molecular ion ([M+H]$^+$) at m/z 315. A linear relationship for MDL was found in the range of 2.5${\sim}$100 ng/ml. The lower limit of quantitation (LLOQ) was 2.5 ng/ml with acceptable precision and accuracy. The intra- and inter-day validation for all coefficients of variation (R.S.D.%) were found less than 15%. Main pharmacokinetic parameters of 30 mg of nicergoline were revealed as follows: AUC$_t$ 321.1${\pm}$64.5 ng${\cdot}$hr/ml, C$_{max}$, 51.2${\pm}$25.3 ng/ml, T$_{max}$ 3.6${\pm}$1.5 hr, K$_{el}$ 0.12${\pm}$0.07 hr$^{-1}$ and t$_{1/2}$ 7.6${\pm}$3.4 hr. Inter subject variations and race differences were shown in comparison with the published data in the literature.

• The Sea:JOURNAL OF THE KOREAN SOCIETY OF OCEANOGRAPHY
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• v.17 no.4
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• pp.243-251
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• 2012

Real-time monitoring for environmental factors(temperature, salinity, chlorophyll, etc.) and carbonate components( pH and $fCO_2$) was conducted during 5-6th of July, 2012 at a seaweeds farm in Gijang, Busan. Surface temperature and salinity were ranged from $12.5{\sim}17.6^{\circ}C$ and 33.7~34.0, respectively, with highly daily and inter-daily variations due to tide, light frequency(day and night) and currents. Surface $fCO_2$ and pH showed a range of $381{\sim}402{\mu}atm$ and 8.03~8.15, and chlorophyll-a concentration in surface seawater ranged 0.8~5.8 ${\mu}g\;L^{-1}$. Environmental and carbonate factors showed the highest/lowest values around 5 pm of 5th July when the lowest tidal height and strongest thermocline in the water column, suggesting that biological production resulted in decrease of $CO_2$ and increase of pH in the seaweed farm. Processes affecting the surface $fCO_2$ distribution were evaluated using a simple budget model. In day time, biological productions by phytoplankton and macro algae are the main factors for $CO_2$ drawdown and counteracted the amount of $CO_2$ increase by temperature and air-sea exchange. The model values were a little higher than observed values in night time due to the over-estimation of physical mixing. The model suggested that algal production accounted about 14-40% of total $CO_2$ variation in seaweed farm.

• Journal of Ginseng Research
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• v.37 no.1
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• pp.135-141
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• 2013

A rapid, sensitive and selective analytical method was developed and validated for the determination of compound K, a major intestinal bacterial metabolite of ginsenosides in human plasma. Liquid-liquid extraction was used for sample preparation and analysis, followed by liquid chromatography tandem spectrometric analysis and an electrospray-ionization interface. Compound K was analyzed on a Phenomenex Luna C18 column ($100{\times}2.00$ mm, 3 ${\mu}m$) with the mobile phase run isocratically with 10 mM ammonium acetate-methanol-acetonitrile (5:47.5:47.5, v/v/v) at a flow rate of 0.5 mL/min. The method was validated for accuracy (relative error <12.63%), precision (coefficient of variation <9.14%), linearity, and recovery. The assay was linear over the entire range of calibration standards i.e., a concentration range of 1 ng/mL to 1,000 ng/mL ($r^2$ >0.9968). The recoveries of compound K after liquid-liquid extraction at 1, 2, 400, and 800 ng/mL were $106.00{\pm}0.08%$, $103.50{\pm}0.19%$, $111.45{\pm}5.21%$, and $89.62{\pm}34.46%$ for intra-day and $85.40{\pm}0.08%$, $94.50{\pm}0.09%$, $112.50{\pm}5.21%$, and $95.87{\pm}34.46%$ for inter-day, respectively. The lower limit of quantification of the analytical method of compound K was 1 ng/mL in human plasma. The developed method was successfully applied to a pharmacokinetic study of compound K after oral administration in ten of healthy human subjects.

• Biomolecules & Therapeutics
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• v.9 no.4
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• pp.291-297
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• 2001

The bioequivalence of two triflusal products was evaluated with 20 healthy volunteers following single oral dose according to the guidelines of Korea Food and Drug Administration (KFDA). Trisa $l^{R}$ capsule (Whanin Pharm. Corp., Korea) and Disgre $n^{R}$ capsule (Myung-In Pharm. Corp., Korea) were used as test product and reference product, respectively. Both products contain 300 mg of trifusal. One capsule of test product or reference product was orally administered to the volunteers, respectively, by randomized two period crossover study (2$\times$2 Latin square method). Blood samples were taken at predetermined time intervals for 4 hours and the determination of trifusal was accomplished using semi-microbore HPLC equipped with automated column switching system. The analytical method with HPLC was validated according to the Bioanalytic Method Validation guideline by F7A prior to determining the plasma samples. The pharmacokinetic parameters (AU $C_{0-4h}$ $C_{max}$ and $T_{max}$) were calculated and ANOVA test was utilized for statistical analysis of parameters. As a result of the assay validation, the limit of quantification of trifusal in human plasma by current assay procedure was 50 ng/ml using 500 $\mu$l of plasma. The accuracy of the assay was from 97.76% to 116.51% while the intra-day and inter-day coefficient of variation of the same concentration range was less than 15%. Average drug concentration at the designated time intervals and pharmacokinetic parameters calculated were not significantly different between two products (p>0.05). The difference of mean AU $C_{olongrightarrow4hr}$, $C_{max}$, and $T_{max}$ between the two products (2.92, 4.39, and -2.44%, respectively) were less than 20%. The power (1-$\beta$) and treatment difference ($\Delta$) for AU $C_{olongrightarrow4hr}$ and $C_{max}$ were more than 0.8 and less than 0.2, respectively. Although the power for $T_{max}$ was under 0.8, $T_{max}$ of the two products was not significantly different from each other (p>0.05). These results satisfied the criteria of KFDA guideline for bioequivalence, indicating the two products of triflusal were bioequivalent.quivalent.ent.ent.