• Journal of the Korean Society of Tobacco Science
• /
• v.31 no.1
• /
• pp.45-50
• /
• 2009

In this study, a simple gradient RRLC method for rapid determination of carbonyl compounds of cigarette smoke was developed. Within 10 min, 8 carbonyl compounds have been separated and identified on ZORBAX Eclipse XDB-C18 column ($4.6{\times}50\;mm$, $1.8\;{\mu}m$) with gradient elution using water and acetonitrile as a mobile phase. RRLC was used for the quantification of carbonyl compounds in mainstream smoke of 3R4F reference cigarette, and evaluated those efficiencies in the recovery, repeatability and reproducibility. The correlation coefficients ($r^2$) for calibration curves of carbonyl compounds were over 0.9998. The developed RRLC method was successfully applied to the analysis of smoke samples and the recoveries of carbonyl compounds were in the range of 97.5~102.1% with RSD<3.1%.

• Natural Product Sciences
• /
• v.21 no.3
• /
• pp.192-195
• /
• 2015

An antibacterial benzoquinone, 2,6-dimethoxy-1,4-benzoquinone, isolated from Ficus foveolata stems was used as a standard marker for establishment of quantitative HPLC analysis for the stem extracts of F. foveolata. The method utilized a TSK-gel ODS-80Ts column (5 μm, 4.6 × 250 mm) with the mixture of methanol and 5% acetic acid in water (24:76, v/v) as the mobile phase at a flow rate of 1 mL/min, and quantitative detection at 289 nm. The parameters i.e. linearity, intraday and interday precision, accuracy, specificity and sensitivity of the method were evaluated for method validation. The recoveries of the method were 99.5 - 103.6% and good linearity (R² ≥ 0.9999) was obtained. A high degree of specificity, sensitivity as well as repeatability and reproducibility (RSD less than 2 and 5%, respectively) were also achieved. Chloroform was served as the most suitable solvent for extraction of 2,6-dimethoxy-1,4-benzoquinone. The optimised sample preparation and HPLC method can be practically used in the routine quality control process of F. foveolata stem extracts.

• Korean Journal of Pharmacognosy
• /
• v.43 no.4
• /
• pp.286-290
• /
• 2012

Many diterpenoids from Siegesbeckia species (Compositae) and their anti-inflammatory actions have been examined. In this research, high-performance liquid chromatography-ultraviolet spectrophotometer (HPLC-UV) method was used to compare the quantitative level of kirenol (ent-pimarane-type diterpenoid) in the aerial parts of Korean S. glabrescens and S. pubescens and the Chinese Siegesbeckiae Herba. Fingerprints of the two HPLC chromatograms of Korean S. glabrescens and S. pubescens were similar, but considerably different from Chinese Siegesbeckiae Herba. The content of kirenol in S. pubescens ($16.51{\pm}0.10$ mg/ml dry weight as mean${\pm}$RSD) was higher than S. glabrescens ($13.48{\pm}0.12$ mg/g dry weight). These values were considerably higher than the Chinese Siegesbeckiae Herba ($1.55{\pm}0.74$ mg/g dry weight). Thin layer chromatography (TLC) analysis demonstrated the containing of kirenol in the three plant materials, but the presence of siegeskaurolic acid (entkaurane-type diterpenoid) only in the Chinese Siegesbeckiae Herba.

• Proceedings of the Korean Society of Soil and Groundwater Environment Conference
• /
• 2005.04a
• /
• pp.308-311
• /
• 2005

[ $^{222}Rn\;and\;^{226}Ra$ ] in groundwater were determined simultaneously using a gamma-spectroscopy. A nitrogen flushing equipment has been used for elimination and stabilization of high and unstable background activity due to the radon and its progenies in counting shield and room. The aim of present work was to control the background activity for simultaneous measurement of radium$(^{226}Ra)$ and radon$(^{222}Rn)$ in groundwater using a gamma-spectrometry. Background activity was about 1.0dps and the standard deviation was about 50%, The background activity could be minimized using nitrogen flushing equipment in the range of 0.1 to 0.5 and the RSD was about 5% at the experimental condition. The detection limit of $^{222}Rn\;and\;^{226}Ra$ in groundwater was 0.5dps/L in the background control method. In most groundwater used in the work, radon activity was more than the detection limit. However, radium activity in some groundwater was less than the detection limit. If the low level radium in groundwater must be measured, preconcentration process such as concentration should be performed before measuring the groundwater.

• Food Science and Biotechnology
• /
• v.18 no.2
• /
• pp.561-564
• /
• 2009

A high performance liquid chromatography (HPLC) method has been developed for determination of 11 ginsenosides in black ginseng (BG, white ginseng that is subjected to 9 cycles of $95^{\circ}C$ for 3 hr). After eluted by gradient elution of water-acetonitrile without buffer in 70 min, 11 ginsenosides in BG were identified. The proposed method provided good linearity ($R^2$>0.9995), accuracy (92.2-106.6%), and intra- and interday precision (RSD<2.6%). In addition, ginsenosides compositions in white, red, and black ginsengs were investigated using this method, respectively. Interestingly, in BG, the content of ginsenoside $Rg_3$ which does not existed in white ginseng was 7.51 mg/g, approximately 20 times than that in red ginseng.

• Food Science and Biotechnology
• /
• v.18 no.5
• /
• pp.1118-1123
• /
• 2009

Event-specific real-time polymerase chain reaction (PCR) detection method for genetically modified (GM) maize MIR604 was developed based on integration junction sequences between the host plant genome and the integrated transgene. In this study, 2 primer pairs and probes were designed for specific amplification of 100 and 111 bp DNA fragments from the zSSIIb gene (the maize endogenous reference gene) and MIR604. The quantitative method was validated using 3 certified reference materials (CRMs) with levels of 0.1, 1, and 10% MIR604. The method was also assayed with 14 different plants and other GM maize. No amplification signal was observed in real-time PCR assays with any of the species tested other than MIR604 maize. As a result, the bias from the true value and the relative deviation for MIR604 was within the range from 0 to 9%. Precision, expressed as relative standard deviation (RSD), varied from 2.7 to 10% for MIR604. Limits of detections (LODs) of qualitative and quantitative methods were all 0.1%. These results indicated that the event-specific quantitative PCR detection system for MIR604 is accurate and useful.

• Journal of Korean Society for Atmospheric Environment
• /
• v.8 no.3
• /
• pp.155-161
• /
• 1992

A simple, fast yet sensitive method is described for the determination of fifty elements in coal by inductively coupled plasma mass spectrometry. The method involves complete dissolution of coal with mixed acid $(HNO_3, HF, HClO_4)$ in hish pressure Teflon bomb and subsequent inductively coupled plasma mass spectrometric(ICP-MS) measurement. The accuracy of the method, being evaluated by the analysis of NIST SRMs (1632a, 1632b) is better than 20% RSD for most elements. The limits of detection defined by two times $\sigma$ (standard deviation of operational blank) are in order of sub-ppm to ppm, which are low enough to quantitate most elements. However, the determiantions for few elements such as V, As, Se are severely interfered by molecular ions such that their accurate determiantions are not possible. Analytical results for twentyon coals from eight countries including six ones world major coal producing, Korea, Japan, China, I.C.S., U.S.A., Canada, Australia, and South Africa are presented. While the results for major elements agree well with the existing ones, those for a few trace elements disagree considerably. The existing values are considerably higher. It is not possible to judge which are more accurate. However, the exisisting values are more likely to be errorous inasmuch as they are obtained without using high purity reagents and clean laboratory techniques.

• Bulletin of the Korean Chemical Society
• /
• v.33 no.1
• /
• pp.171-176
• /
• 2012

A novel chemiluminescence (CL) system was established for the determination of cytosine arabinoside (Ara-C) in pharmaceutical preparations. It was showed that a clear CL signal was observed when Eosin Y mixed with Fenton reagent. The CL intensity was decreased significantly when Ara-C was added to the reaction system and partially scavenged the hydroxyl radicals in the solution. The extent of decrease in the CL intensity had a good stoichiometrical relationship with the Ara-C concentration. Based on this, we developed a new method for the determination of Ara-C using a flow injection analysis (FIA) technique with CL detection. Under the optimal conditions, the linear range of Ara-C concentration was $6.0{\times}10^{-9}\sim1.0{\times}10^{-7}mol/L$ (R = 0.9982) with a detection limit of $7.6{\times}10^{-10}mol/L$ (S/N=3), the RSD was 5.6% for $6.0{\times}10^{-8}mol/L$ Ara-C (n = 11). The method was successfully applied to the determination of Ara-C in injection samples. The possible chemiluminescence reaction mechanism was discussed.

• 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.34 no.11
• /
• pp.3239-3242
• /
• 2013

An improved rapid method for determination of the fatty acid composition using modified methylation procedure was compared with the AOAC reference procedure based on the methylation of fatty acid with the addition of BF3 catalyst before and while heating. The new method is useful for research and routine quality control and has a number of advantages over the reference procedure which are more rapid, simple and also reliable. Applicability of the modified methylation method was confirmed with three vegetable oil samples (palm oil, coconut oil and olive oil). Based on the validation method results, we obtained that a quite linear calibration curve of fatty acids was performed with $R^2$ in range of 0.9972-0.9994. The sensitivity of gas chromatography instrument was able to analyze the fatty acids up to a few ppm, the precision and accuracy were good enough with the %RSD between 1.5%-19.5% and the recovery of linolenic acid was 99.1% in the range of 80.0%-113.3%.