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

• Journal of the Society of Cosmetic Scientists of Korea
• /
• v.40 no.1
• /
• pp.37-44
• /
• 2014

Preservatives such as paraben, phenoxyethanol, and chlorphene are commonly used in cosmetics thanks to cheap price and good antiseptic effect. Recently, consumers' concerns about their possible toxicity and skin irritation forced them to be replaced with straight 1,2-alkanediols. However, as the alkanediols may also irritate skin, limited amount of them should be used in cosmetics. Three 1,2-alkanediols including 1,2-pentanediol, 1,2-hexanediol, and 1,2-octanediol in cosmetics were analyzed simultaneously by gas chromatogrphy with flame ionization detector. As a result of method validation, the specificity was confirmed by the calibration curves of 1,2-pentanediol, 1,2-hexanediol, and 1,2-octanediol showing good linearity correlation coefficient of above 0.999 over the concentration range of $100{\sim}1,200{\mu}g/g$. The limit of detection (LOD) and quantification (LOQ) of 1,2-pentanediol, 1,2-hexanediol, and 1,2-octanediol were 31, 40, and $19{\mu}g/g$ and 98, 108, and $57{\mu}g/g$, respectively. The precision (Repeatability) of the amount in cosmetics showed less than 2.0%. Relative Standard Deviation (% RSD) and the Accuracy (% recovery) of the amount in cosmetics showed 99.3 ~ 103.3, 99.4 ~ 106.7, 97.5 ~ 107.3% respectively. As a result, simultaneous analysis of antimicrobial three 1,2-alkanediols in cosmetics were possible. This method can be utilized in accurate quantitative analysis of 1,2-alkanediols in cosmetics.

• Journal of Radiation Protection and Research
• /
• v.20 no.4
• /
• pp.275-283
• /
• 1995

PERALS(Photon Electron Rejecting Alpha Liquid Scintillation) spectrometry coupled with solvent extraction method has been set up for the analysis of $^{222}Rn\;and\;^{226}Ra$ in the groundwater. This analytical method offers low background, better energy resolution and lower quenching problem than the other techniques. By the analysis of NIST SRM 4966 $^{226}Ra$ standard, the analytical accuracy and precision were found to be 3% and 1%, respectively, and the relative standard deviation of the recovery of Rn extraction between pH2 and pH10 was 7%. Detection limits of $^{222}Rn$ and $^{226}Ra$ for 10 hours counting were counted to be $0.42 pCi/{\iota}\;and\;0.016 pCi/{\iota}$, respectively. For the test analysis of $^{222}Rn\;and\;^{226}Ra$ in the graundwater, hot spring water samples of 17 regions were analyzed. The concentration of $^{222}Rn$ were in the range of $90{\sim}5200pCi/{\iota}$ and average value was $1470pCi/{\iota}\;^{226}Ra$ concentration showed a peak value of $97.9pCi/{\iota}$ in a Kangwon region, but the average value was $1.14pCi/{\iota}$ except that region.

• Journal of Korean Society for Atmospheric Environment
• /
• v.23 no.5
• /
• pp.547-556
• /
• 2007

The release, sampling and analytical methods have been developed and tested for perfluorocarbons (PFCs) atmospheric tracers in order to gain insight into the atmospheric transport and dispersion over the urban conditions of Seoul, Korea. Although PFCs tracer experiments provide unique opportunities to test local and urban scale of transport and dispersion, no previous experiment with PFCs has been conducted in Korea. PMCH and PDCH were chosen as targeted tracers in our study due to their extreme low ambient concentrations and great sensitivities among various PFCs. For PFCs release system, a set of micro-metering pump, electronic balance, vaporizing furnace and high speed blower was constructed for precise and accurate release of tracers. The precision of released rate by this system was estimated to be 1%. Samplings of PFCs were carried out by fabricated portable air samplers with micro pumps and rotameters into glass tubes packed with 150 mg of Carboxen-569. The uncertainty of these sampling system was maintained below 14%. PMCH and PDCH were quantified in GC/ECD with preconditioned injection system to eliminate the interference compounds using traps and subsequent catalytic conversion system prior to column separation. Three intensive field test were undertaken during the springtime of 2002 to 2004 in eastern part of Seoul. Daily background samples were collected to characterize the background levels of PMCH and PDCH prior to their release. The observed background concentrations of PMCH ranged from 3.5 to 10.1 fL/L and varied randomly in location and time in this study. Its mean and standard variation of background concentration ($6.8{\pm}1.9\;fL/L$) are higher than those ($3.2{\sim}5.8\;fL/L$) of other historic tracer studies. Identified uncertainty for background PMCH was $1.7{\sim}2.0\;fL/L$ using this analytical system. Combined relative uncertainty in determining the tracer's concentrations was estimated as 17%. However, its background concentrations and uncertainty in concentration determination were found to be low and stable enough for tracer study.

• Journal of Pharmaceutical Investigation
• /
• v.36 no.1
• /
• pp.45-51
• /
• 2006

A rapid, selective and sensitive reversed-phase HPLC method for the determination of dipyridamole in human serum was developed, validated, and applied to the pharmacokinetic study of dipyridamole. Dipyridamole and internal standard, loxapine, were extracted from human serum by liquid-liquid extraction with diethyl ether and analyzed on a Nova Pak $C_{I8}$ column with the mobile phase of 40 mM ammonium acetate:methanol:acetonitrile (35:35:30)(v/v/v, pH 7.8). Detection wavelength of 280 nm and flow rate of 1.0 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^3$ factorial design using a fixed dipyridamole concentration (50 ng/mL) with respect to its peak area and retention time. And also, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 2-2000 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 0.5 mL of serum was 2 ng/mL, which was sensitive enough for pharmacokinetic studies of dipyridamole. The overall accuracy of the quality control samples ranged from 103.94 to 105.86% for dipyridamole with overall precision (% C.V.) being 4.60-11.49%. The relative mean recovery of dipyridamole for human serum was 97.64%. Stability studies showed that dipyridamole was stable during storage, or during the assay procedure in human serum. The peak area and retention time of dipyridamole were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of dipyridamole in human serum samples for the pharmacokinetic studies of orally administered Dimor tablet (75 mg as dipyridamole) at three different laboratories, demonstrating the suitability of the method.

• Journal of Pharmaceutical Investigation
• /
• v.36 no.1
• /
• pp.23-29
• /
• 2006

A rapid, selective and sensitive reversed-phase HPLC method for the determination of promethazine in human serum was developed, validated, and applied to the pharmacokinetic study of promethazine. Promethazine and internal standard, chlorpromazine, were extracted from human serum by liquid-liquid extraction with n-hexane containing 0.8% isopropanol and analyzed on a Capcell Pak CN column with the mobile phase of acetonitrile-0.2 M potassium dihydrogen phosphate (42:58, v/v, adjusted to pH 6.0 with 1 M NaOH). Detection wavelength of 251 nm and flow rate of 0.9 mL/min were fixed for the study. The assay robustness for the changes of mobile phase pH, organic solvent content, and flow rate was confirmed by $3^{3}$ factorial design using a fixed promethazine concentration (10 ng/mL) with respect to its peak area and retention time. In addition, the ruggedness of this method was investigated at three different laboratories using same quality control (QC) samples. This method showed linear response over the concentration range of 1-40 ng/mL with correlation coefficients greater than 0.999. The lower limit of quantification using 1 mL of serum was 1 ng/mL, which was sensitive enough for pharmacokinetic studies. The overall accuracy of the quality control samples ranged from 96.15 to 105.40% for promethazine with overall precision (% C.V.) being 6.70-11.22%. The relative mean recovery of promethazine for human serum was 63.54%. Stability (freeze-thaw and short-term) studies showed that promethazine was stable during storage, or during the assay procedure in human serum. However, the storage at $-80^{\circ}C$ for 4 weeks showed that promethazine was not stable. Extracted serum sample and stock solution were not allowed to stand at ambient temperature for 12 hr prior to injection. The peak area and retention time of promethazine were not significantly affected by the changes of mobile phase pH, organic solvent content, and flow rate under the conditions studied. This method showed good ruggedness (within 15% C.V.) and was successfully used for the analysis of promethazine in human serum samples for the pharmacokinetic studies of orally administered Himazin tablet (25 mg as promethazine hydrochloride) at three different laboratories, demonstrating the suitability of the method.

• The Korean Journal of Pesticide Science
• /
• v.14 no.1
• /
• pp.21-29
• /
• 2010

The analytical method for bifenazate was developed using a HPLC (UVD). Also, analytical condition of LC/MS was set up for bifenazate. We validated the method for the precision and the reproducibility. The correlation coefficient of bifenazate ranged from 0.05 to 2.5 mg/kg was 1.0. Limit of quantitation (LOQ) was 0.01 mg/kg. To measure recoveries from agricultural products such as foxtail millet (cereal grains), kidney bean (beans), orange (fruits), perilla leaves (vegetables) and oak mushroom (mushrooms), bifenazate was spiked. Mean recoveries of bifenazate for each sample were 82.7~104.1% at the level of 0.1 mg/kg and 73.1~104.3% at the level of 0.5 mg/kg. The relative standard deviations (n=3) were 0.2~9.7%. Pesticide residues for bifenazate were investigated in 16 commodities (rice, foxtail millet, buckwheat, kidney bean, peanut, sesame, orange, grapefruit, kiwifruit, spinach, perilla leaves, leek, garlic stem, garlic, ginger and oak mushroom) collected from 22 provinces in 2009. Bifenazate was analyzed using analytical method by HPLC from 304 samples, and residue was not detected.

• Applied Chemistry for Engineering
• /
• v.25 no.2
• /
• pp.121-133
• /
• 2014

Block copolymers including ABA triblock architectures are useful as thermoplastic elastomers and toughened plastics depending on the relative glassy and rubbery content. These materials can be blended with other polymers and utilized as additives, toughening agents, and compatibilizers. Most of commercially available block copolymers are derived from petroleum. Renewable alternatives are attractive considering the finite supply of fossil resources on earth and the overall economic and environmental expenses involved in the recovery and use of oil. Furthermore, tomorrow's sustainable materials are demanding the design and implementation with programmed end-of-life. The present review focuses on the preparation and evaluation of new classes of renewable ABA triblock copolymers and also emphasizes on the use of carbohydrate-derived poly(lactide) or plant-based poly(olefins) having a high glass transition temperature and/or high melting temperature for the hard phase in addition to the use of bio-based amorphous hydrocarbon polymers with a low glass transition temperature for the soft components. The combination of multiple controlled polymerizations has proven to be a powerful approach. Precision-controlled synthesis of these hybrid macromolecules has led to the development of new elastomers and tough plastics offering renewability, biodegradability, and high performance.

• Journal of Pharmaceutical Investigation
• /
• v.40 no.2
• /
• pp.101-107
• /
• 2010

A rapid and sensitive reversed-phase high performance liquid chromatography (HPLC) method was developed for the determination of N-(-4-Chlorophenyl)-6-hydroxy-7-methoxy-2-chromanecarboxamide (KAL-1120), a novel anti-inflammation agent, in the rat plasma. The method was applied to analyze the compound in the biological fluids such as bile, urine and tissue homogenates. After liquid-liquid extraction, the compound was analyzed on an HPLC system with ultraviolet detection at 275 nm. HPLC was carried out using reversed-phase isocratic elution with a $C_{18}$ column, a mobile phase of a mixture of acetonitril (40 v/v%) at a flow rate of 1.0 mL/min. The chromatograms showed good resolution and sensitivity and no interference of plasma. The calibration curve for the drug in plasma was linear over the concentration range of 0.05-50 ${\mu}g$/mL. The intra- and inter-day assay accuracies of this method ranged from 0.06% to 9.33% of normal values and the precision did not exceed 6.28% of relative standard deviation. The plasma concentration of KAL-1120 decreased to below the quantifiable limit at 1.5 hr after the i.v. bolus administration of 2-10 mg/kg to rats ($t_{1/2,({\alpha})}$ and $t_{1/2,({\beta})$ of 2.15 and 26.7 min at a dose of 2 mg/kg, 3.91 and 33.0 min at a dose of 10 mg/kg, respectively). The steady-state volume of distribution ($V_{dss}$) and the total body clearance ($CL_t$) were not significantly altered in rats given doses from 2 to 10 mg/kg. Of the various tissues tested, KAL-1120 was mainly distributed in the lung and heart after i.v. bolus administration. KAL-1120 was detected in the bile by 30 min after its i.v. bolus administration. However, the concentration in the urine after i.v. bolus administration became too low to measure, suggesting that KAL-1120 is mostly excreted in the bile. In conclusion, this analytical method was suitable for the preclinical pharmacokinetic studies of KAL-1120 in rats.

• Journal of Food Hygiene and Safety
• /
• v.30 no.2
• /
• pp.173-177
• /
• 2015

Rosa canina L. is health functional food materials that can help to temporarily relieve symptoms of arthritis. This study has been conducted to develop and validate analytical methods for hyperoside of Rosa canina L.. Methods based on HPLC with ultraviolet detection (UVD) were established through instrumental analytical conditions, and the examination of data, such as domestic and foreign reliable methods and journals. HPLC UVD analysis using Capcell Pak $C_{18}$ MG II column at 353 nm was determined on test through the column, mobile phase. The validation has been performed on the method to determine linearity, accuracy, limits of quantification (LOQ) and repeatability for hyperoside. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.999, and the LOQ was $0.393{\mu}g/mL$. Relative standard deviation (RSD) values of data from repeatability precision was between 0.6 and 2.6%. Recovery rate test at hyperoside scored between 98 and 99%. These results indicate that the established HPLC method is very useful for the determination of hyperoside in Rosa canina L. to develop a health functional material.