• Proceedings of the Korean Society of Applied Pharmacology
• /
• 1998.11a
• /
• pp.123-123
• /
• 1998

A number of uracil derivatives have been developed as anti-AIDS drugs having a mechanism of inhibiting cellular reverse transcriptase. A simple and rapid assay technique for recently synthesized KR-V analogues was developed using a high-performance liquid chromatography, and oral pharmacokinetics was examined for assessing their oral bioavailabilites. Plasma samples were analyzed by reversed-phase HPLC using an ODS column with an ultraviolet detection system. All the analogues were eluted within 12 min and the LOQ was 15-30 ng/$m\ell$. The extraction recoveries were higher than 85%, except KR-V1039, 1068 and 1720 having ester group. This chromatic method was well applied to the kinetic studies for KR-V analogues. Among 16 analogues tested in the present work, the 6 compounds including KR-V1123, 1122, 1784, 1783, 1736 and 1700 were found to be bioavailable for oral administration to rats.

• Journal of Korean Society of Occupational and Environmental Hygiene
• /
• v.16 no.2
• /
• pp.91-100
• /
• 2006

The purpose of this study was to validate alternative method by using non-carcinogenic, and less toxic solvents than NIOSH analytical method 5524 for measuring the airborne MWFs in workplaces. In laboratory tests, the ETM solvents(mixture of same volume for ethyl ether, toluene, and ethanol) were selected. The alternative method of analyzing MWFs, referred to as the ETM solvent extraction method, showed 0.04 mg/sample as LOD, and 0.15 mg/sample as LOQ. The analytical precision (pooled CV, coefficient of variation) of the ETM solvent extraction method for analyzing the straight, soluble, semisynthetic, and synthetic metalworking fluid was 1.5%, 2.0%, 2.6%, 1.6%, respectively, which was similar to the precision (2.6%) of NIOSH analytical method (NIOSH 0500) for total dust. The analytical accuracy by recovery test, spiked mass calculated as extractable mass, was almost 100%. As the result of storage stability test, metalworking fluid samples should be stored in refrigerated condition, and be analyzed in two weeks after sampling. The 95% confidence limit of the estimated total standard error for the ETM solvent extraction method for analyzing the straight, soluble, semisynthetic, and synthetic metalworking fluid was ${\pm}12.6%$, ${\pm}12.5%$, ${\pm}14.0%$, and ${\pm}13.6%$, respectively, which satisfied the OSHA sampling and analytical criteria.

• Bulletin of the Korean Chemical Society
• /
• v.35 no.1
• /
• pp.197-203
• /
• 2014

A rapid, accurate and precise method for the determination of 22 amino acids in Isatidis Radix by Hydrophilic Interaction Ultra-High-Performance Liquid Chromatography Coupled with Triple-Quadrupole Mass Spectrometry (HILIC-UPLC-MS/MS) was established. Chromatographic separation was carried out on a Acquity UPLC BEH Amide column ($2.1mm{\times}100mm$, $1.7{\mu}m$) with gradient elution of acetonitrile (containing 0.05% formic acid and 2 mM ammonium formate) and water (containing 0.15% formic acid and 10 mM ammonium formate) at a flow rate of 0.4 mL/min; Waters Xevo$^{TM}$ TQ worked in multiple reaction monitoring mode. All components were separated in 17 min. All calibration curves were linear ($R^2$ > 0.991) over the tested ranges. The limits of detection (LOD) and limits of quantitation (LOQ) for these compounds were 0.21-79.55 and 0.72-294.23 ng/mL, respectively. The average recoveries were in the range of 93.75-104.16% with RSD value less than 6.56%. Therefore, this method could be an alternative assay for the determination of 22 amino acids in Isatidis Radix due to its rapidness, sensitivity, less sample and solvent consumption.

• Bulletin of the Korean Chemical Society
• /
• v.32 no.10
• /
• pp.3603-3609
• /
• 2011

A novel sampling method of the headspace poly(dimethylsiloxane) (PDMS) mini-disk extraction (HS-PDE) was developed, optimized, validated and applied for the GC/MS analysis of spices flavors. A prototype PDMS mini-disk (8 mm outer diameter, 0.157 mm thickness, 9.4 mg weight) has been designed and fabricated as a sorption device. The technique uses a small PDMS mini-disk and very small volume of organic solvent and less sample size than the solvent extraction. This new HS-PDE method is very simple to use, inexpensive, rapid, requires less labor. Linearities of calibration curves for ${\alpha}$-pinene, ${\beta}$-pinene, limonene and ${\gamma}$-terpinene by HS-PDE combined with GC/MS were excellent having $r^2$ values greater than 0.99 at the dynamic range of 6.06~3500 ng/mL. The limit of detection (LOD) and the limit of quantitation (LOQ) showed very low values. This method exhibited good precision and accuracy. The overall extraction efficiency of this method was evaluated by using partition coefficients ($K_p$) and concentration factors (CF) for several characteristic components from nutmeg and mace. Partition coefficients were in the range from $2.04{\times}10^4$ to $4.42{\times}10^5$, while CF values were 0.88-15.03. HS-PDE was applied successfully for the analysis of flavors compositions from nutmeg, mace and cumin. The HS-PDE method is a very promising sampling technique for the characterization of volatile flavors.

• Bulletin of the Korean Chemical Society
• /
• v.30 no.11
• /
• pp.2675-2679
• /
• 2009

This paper reports the example of headspace mulberry paper bag micro solid phase extraction (HS-MPB-$\mu$-SPE) as a new sampling method for the determination of volatile flavor composition of coriander seeds. Adsorption efficiencies between two configurations of mulberry paper bag were compared, and several parameters affecting the HS-MPB-$\mu$-SPE were investigated and optimized. The optimized technique uses an adsorbent (Tenax TA, 0.1 mg) contained in a mulberry paper bag of front configuration where fine surface was outside, and minimal amount of organic solvent (0.6 mL). Linalool and $\gamma$-terpinene were found as abundant flavor compounds from coriander seeds. The limit of detection (LOD) and the limit of quantitation (LOQ) for linalool of major flavor in coriander seeds were 10.3 ng/mL and 34.4 ng/mL, respectively. The proposed method showed good reproducibility and good recovery. The HS-MPB-$\mu$-SPE is very simple to use, inexpensive, requires small sample amounts and solvent consumption. Because the solvent for extraction is reduced to only a very small volume, there is minimal waste or exposure to toxic organic solvent and no further concentration step.

• Journal of agriculture & life science
• /
• v.46 no.6
• /
• pp.165-171
• /
• 2012

As a preceding study for investigating the influence of sound wave stimulus on Arabidopsis thaliana metabolomics, the polar secondary metabolomes of the plant were determined using high performance liquid chromatography coupled with tandem mass spectrometry. A total of 10 polar secondary metabolomes were characterized and quantified. Among them, 4 metabolomes, p-coumaroylagmatine isomer (7 and 8), p-coumaroylagmatine isomer (9 and 10) were identified in the plant for the first time. The validation was conducted in terms of linearity, recovery, precision, limit of detection (LOD) and limit of quantification (LOQ). The validated method was applied to the simultaneous quantification of the 10 polar secondary metabolomes.

• Korean Journal of Pharmacognosy
• /
• v.50 no.2
• /
• pp.133-140
• /
• 2019

In our previous study, we found uracil, adenosine, protocatechuic acid, syringin (eleutheroside B) and scoparone (6, 7-dimethoxycoumarin) in the Oplopanax elatus Nakai Stem. High-performance liquid chromatography (HPLC) -UV was used to quality and quantify the internal marker compounds in the O. elatus extract after validation of method with linearity, limit of detection (LOD), limit of quantitation (LOQ), accuracy and precision. The specificity assessment visually confirmed that the substance was detected without the introduction of other substances. The established method showed high linearity of the calibration curve and coefficient of correlation ($R^2$) of over the 0.999. HPLC was reported as five standard compounds equivalent using the following linear equation based on the calibration curve. The accuracy of measurement was 84.34 ~ 119.74% and the relative standard deviation (RSD) value was 0.28 ~ 1.60%. In addition, our established method showed high repeatability. The RSD value was 1.10 ~ 6.81%. So, we found the amount of the internal marker compounds in the O. elatus extract. These results demonstrated that can be used to quality evaluation of the O. elatus.

• Safety and Health at Work
• /
• v.12 no.2
• /
• pp.209-216
• /
• 2021

Background: The article presents the results of studies performed in order to develop a new method of airborne potassium bromate(V) determination at workplaces. Methods: The method is based on a collection of the inhalable fraction of potassium bromate(V) using the IOM Sampler, then extraction of bromates with deionized water and chromatographic analysis of the obtained solution. The analysis was performed using ion chromatography with conductometric detection. The tests were performed on a Dionex IonPac®AS22 analytic column (250 × 4 mm, 6 ㎛) with AG22 precolumn (50 × 4 mm 11 ㎛). Results: The method provides for potassium bromate(V) determination within the concentration range of 0.043 ÷ 0.88 mg/m³ for an air sample of 0.72 m³ in volume, i.e., 0.1-2 times the exposure limit value as proposed in Poland. The method was validated in accordance with PN-EN 482. The obtained validation data are as follows: measuring range: 3.1-63.4 ㎍/mL, limit of detection (LOD) = 0.018 ㎍/mL and limit of quantification (LOQ) = 0.053 ㎍/mL. The developed method has been tested in the work environment, on laboratory employees having contact with potassium bromate(V). Conclusion: The analytical method allowed the determination of the inhalable fraction of airborne potassium bromate(V) at workplaces and can be used to assess occupational exposure.

• Journal of Environmental Science International
• /
• v.30 no.8
• /
• pp.673-684
• /
• 2021

Raw leachates from three landfills and treated leachates from two landfills on Jeju Isalnd were analyzed for ten perfluorinated compounds (PFCs) detected in aquaruc environments. The leachates were collected six times in 2014 and 2015. Among the ten PFCs, three were not detected, namely perfluoroundecanoic acid (PFUnDA), perfluorododecanoic acid (PFDoDA), and perfluorodecane sulfonate (PFDS). The total concentrations of PFCs ranged as 724-3313 ng/L (mean 1999 ng/L) in raw leachates and from less than the limit of quantification (LOQ) to 394 ng/L (mean 133.2 ng/L) in treated leachates. The domonant compounds measured were perfluorooctanoic acid (PFOA) (mean contribution 37.7%) and perfluorobutane sulfonate (PFBS) (mean contribution 38.2%) in raw leachates, and PFOA (mean contribution 40.7%), perfluorohexanoic acid (PFHxA) (mean contribution 27.3%) and PFBS (mean contribution 26.5%) in treated leachates. No significant correlations were observed between total/several individual PFCs and leachate pH and COD_Cr, which may be due to complex chemical nature of landfill leachates and characteristics of waste and landfills.

• Food Science of Animal Resources
• /
• v.41 no.5
• /
• pp.816-825
• /
• 2021

This study aims to validate a fast method of simultaneous analysis of 365 LCamenable and 142 GC-amenable pesticides in hen eggs by liquid chromatography-tandem mass spectrometry (LC-MS/MS) and gas chromatography-tandem mass spectrometry (GC-MS/MS), respectively, operating in multiple reaction monitoring (MRM) acquisition modes. The sample preparation was based on quick, easy, cheap, effective, rugged, and safe (QuEChERS) extraction. Key method performance parameters investigated were specificity, linearity, limit of quantification (LOQ), accuracy, precision and measurement uncertainty. The method was validated at two spiking levels (10 and 50 ㎍/kg), and good recoveries (70%-120%) and relative standard deviations (RSDs) (≤20) were achieved for 92.9% of LC-amenable and 86.6% of GC-amenable pesticide residues. The LOQs were ≤10 ㎍/kg for 94.2% of LC-amenable and 92.3% of GC-amenable pesticides. The validated method was further applied to 100 egg samples from caged hens, and none of the pesticides was quantified.