• Proceedings of the PSK Conference
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• 2003.10b
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• pp.239.1-239.1
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• 2003

This study was to develop a quantification method of lisinopril using liquid chromatography tendem mass spectrometry in human plasma. Quntitation of lisinopril by MRM(multiple reaction monitoring) in the electrospray positive mode was validated according to FDA guideline. Extraction of lisinopril and enalapril as internal standard from plasma was perfomed by means solide phase extraction. The calibration curve of lisinopril showed a good linerarity in the concentration range 2∼200ng/ml. The coefficients of variations for the inter-day and intra-day precision was less than 15%, and the inter-day and intra-day accuracy was 97.6∼101.0%. (omitted)

• Natural Product Sciences
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• v.22 no.4
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• pp.238-245
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• 2016

Gumiganghwal-tang has been used for the treatment of common cold for a long-time. We developed an accurate and sensitive high performance liquid chromatography-diode array detection (HPLC-DAD) and electrospray ionization mass spectrometry method for the simultaneous determination of ferulic acid, baicalin, bergapten, methyl eugenol, glycyrrhizin, oxypeucedanin, wogonin, nodakenin, atractylenolide III, imperatorin, and atractylenolide I in Gumiganghwal-tang samples. The analytes were separated on a Shiseido C18 column ($5{\mu}m$, $4.6mm\;I.D.{\times}250mm$) with gradient elution with acetonitrile and 0.1% trifluoroacetic acid. Eleven compounds were quantitatively determined by HPLC-DAD and identified by LC-MS data. We also validated this method. The calibration curves of all the compounds showed good linear regression. The limits of detection and the limits of quantification ranged from 0.04 to 0.63 and from 0.12 to $1.92{\mu}g/mL$, respectively. The relative standard deviation values of intra- and inter-days of this method represented less than 2.9%. The recoveries were found to be in the range of 90.06 - 107.66%. The developed method has been successfully applied to the analysis of Gumiganghwaltang samples. The established HPLC method could be used to quality control of Gumiganghwal-tang.

• Nuclear Engineering and Technology
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• v.28 no.6
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• pp.507-521
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• 1996

Quantification of uncertainties in the source term estimations by a large computer code, such as MELCOR and MAAP, is an essential process of the current Probabilistic safety assessment. The main objective of the present study is to investigate the applicability of a combined procedure of the response surface method (RSM) based on input determined from a statistical design and the Latin hypercube sampling (LHS) technique for the uncertainty analysis of CsI release fractions under a Hypothetical severe accident sequence of a station blackout at Younggwang nuclear power plant using MAAP3. OB code as a benchmark problem. On the basis of the results obtained in the present work, the RSM is recommended to be used as a principal tool for an overall uncertainty analysis in source term quantifications, while using the LHS in the calculations of standardized regression coefficients (SRC) and standardized rank regression coefficient (SRRC) to determine the subset of the most important input parameters in the final screening step and to check the cumulative distribution functions obtained by RSM. Verification of the response surface model for its sufficient accuracy is a prerequisite for the reliability of the final results that can be obtained by the combined procedure proposed in the present work.

• Journal of Korean Institute of Industrial Engineers
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• v.30 no.1
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• pp.44-49
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• 2004

The aim of this study is to compare the methods in analyzing bio-signals representing measure driver's psychophysiological staus. This study has considered three approaches: first, the deterministic approach calculating the mean and standard deviation of bio-signal, second, probabilistic approach converting driver's bio-signal values to probability density function and identifying individual state relative to overall distribution, and third, diagnostic approach identifying the pattern change of signal over certain period of time. For evaluation of analysis methods, driver's bio-signal was collected under various road conditions, and three analysis approaches were applied respectively. In result, the deterministic approach was found to be simple to use, but generated a large variability of bio-signal. The probabilistic approach provide a relative status of individual driver among overall population, but too much affected by temporal variability of individual driver. The diagnostic approach seemed to reasonably find driver's psychophysiological change over certain period of time, but still needs to develop quantification method of the bio-signal.

• Environmental Engineering Research
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• v.23 no.4
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• pp.406-419
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• 2018

In planning public service systems such as waterworks, the design population is very important factor. Owing to the limitations of the indirect method, two new models, which take into consideration urban characteristics, were developed to accurately predict external migration rate (EMR), which is an essential component in estimating reliably the design population. The root mean square error (RMSE) between the model values and observed values were 10.12 and 15.58 for the metropolitan cities and counties respectively and were lower compared to RMSE values of 27.31 and 28.79 obtained by the indirect method. Thus, the developed models provide a more accurate estimate of EMR than the indirect method. In addition, the major influencing factors for external migration in counties were development type, ageing index, number of businesses. On the other hand, the major influencing migration factors for cities were project scale, distance to city center, manufacturing size, population growth rate and residential environment. Future medium and long-term studies would be done to identify emerging trends to appropriately inform policy making.

• Mass Spectrometry Letters
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• v.12 no.2
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• pp.31-40
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• 2021

Probable human carcinogenic compounds nitrosamines, have been detected as by-product impurities in sartan pharmaceuticals in recent years which has drawn worries for medication safety. To provide a sensitive and effective method for the quality control of sartan pharmaceuticals, this study established a feasible gas chromatography-tandem mass spectrometry (GC-MS/MS) method for simultaneous determination of 13 nitrosamines. The target analytes were separated on a DB-WAX Ultra Inert column (30 m × 0.25 mm; i.d., 0.25 ㎛) and were then subjected to electron impact ionization in multiple reaction monitoring mode. The established method was validated and further employed to analyze authentic samples. Limits of detection (LODs) and limits of quantification (LOQs) of the 13 nitrosamines were 15-250 ng/g and 50-250 ng/g, respectively, which also exhibited intra-day and inter-day accuracies of 91.4-104.8%, thereby satisfying validation criteria. Five nitrosamines, viz., N-nitrosodiethylamine, N-nitrosodimethylamine, N-nitrosodiphenylamine, N-nitrosomorpholine, and N-nitrosopiperidine were detected at concentrations above their LODs in 68 positive samples out of 594 authentic samples from seven sartans.

• Journal of Pharmaceutical Investigation
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• v.38 no.1
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• pp.57-61
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• 2008

A HPLC-ELSD method was developed to determine saikosaponin derivatives from Bupleuri Radix. Eight saikosaponins, saikosaponin c, i, h, a, $b_2$, g, $b_1$ and d, were analyzed under optimized HPLC conditions [column: Eclipse XDB $C_{18}$ ($150{\times}4.6mm$ i.d., $5{\mu}m$; mobile phase: $H_2O$ with 0.1% $CH_3$COOH (v/v) for solvent A and AcCN with 0.1% $CH_3$COOH (v/v) for solvent B, gradient elution; flow rate: 1mL/min; injection volume: $20{\mu}L$]. Good linearity was achieved in the range from 62.5 to $250{\mu}g/mL$ for each compound, and intra-day precision and accuracy at each concentration level varied between 0.05 and 5.45% and between 93.9 and 109.6%, respectively, whereas those for inter-day variations were between 0.91 to 2.73% and 94.3 to 106.1%. This HPLC-ELSD method was applied for the determination of sakosaponins from Bupleuri Radix samples, and saikosaponin a $(0.79{\pm}0.20mg/g)$, c $(0.33{\pm}0.06mg/g)$ and d $(0.48{\pm}0.15mg/g)$ were observed as major compounds. The other saikosaponins were shown under limit of quantification level thus couldn't be quantified. The present study suggested that the introduced HPLC-ELSD method is selective and reliable, and not only saikosaponin a, but also saikosaponin c and d should be employed as the standard markers for Bupleuri Radix.

• Korean Journal of Veterinary Service
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• v.43 no.4
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• pp.261-265
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• 2020

Each commercial cyromazine insecticide has different HPLC conditions. The aim of this study was to establish a standardized chromatographic method for the determination of cyromazine in commercial insecticides. The separation was achieved on two C18 columns - Waters® Bondapak C (4×300 nm i.d., 10 ㎛) and X bridge (4.6×250 nm i.d., 5 ㎛) using a mobile phase composed of water/methanol/ethanolamine (76:24:0.1, v/v), with UV detection at wavelengths 230 nm and 254 nm. A total of six commercial cyromazine insecticides were analyzed. In this study, the optimal high-performance liquid chromatography conditions for the analysis of cyromazine were as follows: a mobile phase of water/methanol/ethanolamine (76:24:0.1, v/v) at a flow rate of 1.0 mL/min and a detection wavelength of 230 nm using a X bridge C18 column (4.6×250 nm i.d., 5 ㎛) at a column temperature of 25℃. The calibration curve was linear in the concentration range of 5~50 ㎍/mL, with a correlation coefficient of 0.99995. The cyromazine detection limit was 0.2 ㎍/mL, and the limit of quantification was 0.59 ㎍/mL. The percentage recovery ranged from 99.8% to 101.0% for cyromazine, and the relative standard deviation was not over 2.0%. The cyromazine concentration ranged from 92.7% to 109.4% and was within the acceptable range (90~120%) for the percent of the labeled amount. This method was found to be suitable for determining cyromazine in commercial insecticides.

• KOREAN JOURNAL OF CROP SCIENCE
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• v.56 no.3
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• pp.244-249
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• 2011

A sensitive and rapid high-performance liquid chromatographic-tandem mass spectrometric (HPLC/MS/MS) assay was developed for the determination of soyasaponins in soybean. Among soyasaponins, soyasaponin I was isolated and characterized from methanol extracts of soybean as analytical standards and the development of a new analytical procedure for quantification of its content in various cultivars. The structures of these compound was elucidated by $^1H$, $^{13}C$ NMR experiments and by mass spectrometric analysis. Aqueous ethanol extracts of soybean samples were injected on an Agilent XDB-C18 column ($4.6mm{\times}50mm$, $1.8{\mu}m$) with a mobile phase consisting of 10 mM ammonium acetate-acetonitrile, a flow rate of 0.3 mL/min and a total run time of 8 min. Detection was performed by mass spectrometer bin the multiple reaction monitoring (MRM) mode with negative electrospray ionization (ESI) m/z at 941 ${\rightarrow}$ 615 for soyasaponin I. In the 9 soybean samples, contents of soyasaponin I ranged from 205 to 726 mg/kg, and correlated negatively with seed size.

• YAKHAK HOEJI
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• v.59 no.3
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• pp.98-106
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• 2015

Analytical method for related substances can be categorized into two methods depending on the necessity of reference standard (RS). The analytical method of related substances with RS is fast and accurate, but it's very expensive and technically difficult to synthesize RS due to their complicated structure. Another method is using relative retention time (RRT) and relative response factor (RRF) which are already validated with RS. Validation of this method is not easy and time consuming, but once it has been developed, it can save cost and time. In this study, we developed the analytical method for related substances of fenofibrate using RRT and RRF. We validated the method by evaluating specificity, linearity, accuracy and precision according to the "Manual for Guideline Application for Validation of Analytical Procedures" of MFDS. Also, we calculated RRT and RRF between fenofibrate and fenofibrate related substances. The results of this study showed high specificity for fenofibrate and fenofibrate related substances. Correlation coefficient(r) of all substances were more than 0.99, and the recovery of fenofibrate, fenofibrate related substance I, II and III were 99.44%, 100.84%, 99.14% and 101.58%, respectively. Precision of fenofibrate and its related substances were ranged between RSD 0.29% and 0.93%. Quantification limits of fenofibrate, fenofibrate related substance I, II and III were determined to be $0.03{\mu}g/ml$, $0.05{\mu}g/ml$, $0.04{\mu}g/ml$ and $0.02{\mu}g/ml$, respectively by confirming signal to noise ratio of each chromatogram. The RRT for fenofibrate related substance I, II and III were determined to be 0.35, 0.41 and 1.34, respectively. Also, the RRF for fenofibrate related substance I, II and III were determined to be 1.28, 0.98 and 0.79, respectively. The developed method was applied to determine contents for fenofibrate related substances in commercial fenofibrate (active pharmaceutical ingredient). As a result, developed analytical methods of related substances will be used for revising the monograph of fenofibrate in Korean Pharmacopoeia revision and contribute quality control of drugs by improving cost and time consuming problem of RS.