• The Korea Journal of Herbology
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• v.25 no.3
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• pp.65-71
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• 2010

Objectives：To develop and validate HPLC-PDA methods for simultaneous determination of seven constituents in Samchulkunbi-tang (SKT). Additionally, we investigated the cytotoxicity against BEAS-2B cell line and splenocytes of SKT. Methods：Reverse-phase chromatography using a Gemini $C_{18}$ column operating at $40^{\circ}C$, and photodiode array (PDA) detection at 230, 254 and 280 nm, were used for quantification of the three marker components of SKT. The mobile phase using a gradient flow consisted of two solvent systems. Solvent A was 1.0% (v/v) aqueous acetic acid and solvent B was acetonitrile with 1.0% (v/v) acetic acid. The cytotoxicity of SKT were measured by the CCK-8 assay method. Results：Calibration curves were acquired with $r^2$>0.9999, and the relative standard deviation (RSD) values (%) for intra- and inter-day precision were less than 6.0%. The recovery rate of each compound was in the range of 86.89-109.78%, with an RSD less than 4.0%. The contents of seven compounds in SKT were 1.39-6.84 mg/g. SKT had no cytotoxicity effect at 50-200 ${\mu}g$/mL concentrations. Conclusions：The established method will be helpful to improve quality control and in vitro efficacy study of SKT.

• YAKHAK HOEJI
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• v.54 no.4
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• pp.295-299
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• 2010

The aim of this study was to develop and validate for determination of alibendol in human plasma by HPLC method. After precipitation of 500 ${\mu}l$ plasma samples by 50% methanol 50 ${\mu}l$ and 60% perchloric acid 30 ${\mu}l$ and the supernatant 50 ${\mu}l$ was injected into HPLC. The assay was performed isocratically using 10 mM potassium phosphate (pH 3.0) and acetonitrile (80 : 20, v/v) as mobile phase. The $C_{18}$ column (particle size $3.5{\mu}m$, $4.6{\times}50$ mm, Zorbax Eclipse) was used as a solid phase. The mobile phase was delivered at a flow-rate of 1.7 ml/min, detection was by ultraviolet absorption at 232 nm and concentrations were calculated on the basis of peak areas. In these conditions, alibendol can be separated from ethylparaben, the internal standard, and endogenous substances. The retention times of alibendol and ethylparaben were just about 2.6 and 3.5 minutes, respectively. This rapid HPLC method was validated by examining the precision and accuracy for inter- and intra-day analysis. The standard curve was linear ($R^2$=1.0000) over the concentration range of 0.05~20 ${\mu}g$/ml. The inter-day relative standard deviation (R.S.D.) and accuracy were 0.2~12.2% and 94.4~101.2% (82.7% at the lower limit of quatitation). The intra-day R.S.D. and accuracy were 0.1~11.8% and 98.8~102.5%, respectively. The method was successfully applied to the determination of alibendol in plasma for a pharmacokinetic study.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.27 no.2
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• pp.123-129
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• 2017

Objectives: The purpose of this study is to enhance the application of analytical method of polar solvents(alcohols) by GCOTC (gas chromatography open tubular column) through the system suitability test(SST) to estimate the whole chromatographic system performance(integral part). Methods: To perform the SST, carried out repeatability(n=6) as analytical method of polar solvents by GCOTC, got the retention time($t_R$), standard deviation(${\sigma}_{n-1}$) of $t_R$, baseline width($w_b=4{\sigma}_{n-1}$) and calculated dead time($t_m$) by $v_m=d^2{\pi}L(f/4)$ and $v_m=t_m$ x flow rate. Results: In this experiment, obtained the basic data, there were $t_m=2$ min, methanol($t_R=3.569$, ${\sigma}_{n-1}=0.01$, $w_b=0.04$), ethanol ($t_R=3.892$, ${\sigma}_{n-1}=0.004$, $w_b=0.016$), isopropanol($t_R=4.209$, ${\sigma}_{n-1}=0.004$, $w_b=0.016$). By using these data, calculated the corrected retention time($t_R{^{\prime}}$), capacity factor(k), separation factor(${\alpha}$), number of theoretical plate(n) and resolution($R_s$) for SST and got the good results. Conclusions: Through the SST, could reconfirm the whole chromatographic performance system(integral part) for analytical method of polar solvents by GCOTC. Therefore, this analytical method expect to be widely applied at the related areas.

• Aerospace Engineering and Technology
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• v.3 no.2
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• pp.81-90
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• 2004

This paper describes the results of combustion performance test of fuel-rich gas generator(GG) using LOx and kerosene as propellant at off-design conditions. The chamber pressure is thought to be a function of O/F ratio and total propellant mass flow rate. The test shows that the spatial temperature deviation at the exit of gas generator remains within 7.5K and that the average gas temperature at the exit is a function of propellant O/F ratio. The results of firing test of gas generator at off-design conditions, especially the relation between gas temperature and O/F ratio, can provide useful data for the design of future gas generator and for the development of low-O/F ratio reaction analysis code.

• Bulletin of the Korean Chemical Society
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• v.32 no.2
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• pp.444-450
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• 2011

A novel method that utilizes poly(5-methyl-2-thiozyl methacrylamide-co-2-acrylamido-2-methyl-1-propanesulfonic acid-co-divinylbenzene) [MTMAAm/AMPS/DVB] as a solid-phase extractant was developed for simultaneous preconcentration of trace Cd(II), Co(II), Cr(III), Cu(II), Fe(III), Mn(II), Ni(II), Pb(II), and Zn(II) prior to the measurement by flame atomic absorpiton spectrometry (FAAS). Experimental conditions for effective adsorption of the metal ions were optimized using column procedures. The optimum pH value for the simultaneously separation of the metal ions on the new adsorbent was 2.5. Effects of concentration and volume of elution solution, sample flow rate, sample volume and interfering ions on the recovery of the analytes were investigated. A high preconcentration factor, 100, and low relative standard deviation values, $\leq$1.5% (n = 10), were obtained. The detection limits (${\mu}gL^{-1}$) based on the 3s criterion were 0.18 for Cd(II), 0.11 for Co(II), 0.07 for Cr(III), 0.12 for Cu(II), 0.18 for Fe(III), 0.67 for Mn(II), 0.13 for Ni(II), 0.06 for Pb(II), and 0.09 for Zn(II). The validation of the procedure was performed by the analysis of two certified reference materials. The presented method was applied to the determination of the analytes in various environmental samples with satisfactory results.

• Water for future
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• v.10 no.1
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• pp.53-70
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• 1977

The analysis performed here is aimed to increase the familiarity of hydrologic process especially for the small basins which are densely gaged. Kyung An and Mu Shim river basins are selected as a representative basin according to the criteria which UNESCO has established back in 1964 and being operated under the auspice of Ministry of Construction. The data exerted from these basins is utilized for the determination of characteristics of procipitation and runoff phenomena for the small basin, which is considered as a typical Korean samall watershed. The study found that the areal distribution of preciptation did not show any significant deviation from the point rainfall. Since the area studied is less than 20 km#, the pointrainfall may be safely utilized as a representative value for the area. Also the effect of elevation on the precipitation has a minor significance in the small area where the elevation difference is less than 200m. The methodology developed by Soil Conservation Service for determination of runoff value from precipitation is applied to find the suitability of the method to Korean river basin. The soil cover complex number or runoff curve number was determined by comsidering the type of soil, soil cover, land use and other factors such as antecedent moisture content. The average values of CN for Kyung An and Mushim river basins were found to be 63.9 and 63.1 respectively under AMC II, however, values obtained from soil cover complex were less than those from total precipitation and effective precipitation about 10-30%. It may be worth to note that an attention has to be paid in application of SCS method to Korean river basin by adjusting 10-30% increase to the value obtained from soil cover complex. Finally, the design flood hydrograph was consturcted by employing unit hydrograph technique to the dimensionless mass curve. Also a stepwise multiple regression was performed to find the relationship between runoff and API, evapotranspiration rate, 5 days antecedentprecipitation and daily temperature.

• Natural Product Sciences
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• v.19 no.1
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• pp.20-27
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• 2013

A simple high performance liquid chromatography - diode array detector (HPLC-DAD) method has been developed and validated for simultaneous determination of the six components (cinnamic acid, cinnamaldehyde, eugenol, atractylenolide I, atractylenolide III, and ergosterol) in Oryeongsan. In addition, identification of six marker compounds was conducted by a LC-MS/MS analysis. The six compounds in Oryeongsan were separated on Shishedo $C_{18}$ column (5 ${\mu}m$, $4.6{\times}250$ mm) at a column temperature of $30^{\circ}C$. The mobile phase was a mixture of 0.1% trifluoroacetic acid (TFA) water and acetonitrile employing gradient elution at a flow rate of 1.0 mL/min. The detection wavelength was set at 205, 250, 280, and 330 nm. The developed method had good linearity ($R^2$ > 0.9997) and the limit of detection (LOD) and limit of quantification (LOQ) were observed within the ranges 0.01~0.15 and 0.05~0.45 ${\mu}g/mL$, respectively. The relative standard deviation (RSD) values of intra- and inter-day testing were indicated that less than 3% and 90.31~103.31% of accuracy. The results of recovery test were 90.56~106.72% and RSD range was measured from 0.84 to 2.95%. In conclusion, this HPLC-DAD method has been successfully applied to the simultaneous determination of six compounds in Oryeongsan samples.

• Analytical Science and Technology
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• v.13 no.6
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• pp.781-788
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• 2000

Tellurium in simulated nuclear spent fuels (SIMFUEL) has been determined by hydride generation-inductively coupled plasma atomic emission spectrometry (HG-ICP-AES). Parameters such as concentrations of HCl and $NaBH_4$, flow rate of HCl and $NaBH_4$ were optimized and then the effects of U, Mo, Pd, Rh and Ru on the Te intensity were investigated. A thiourea as a masking agent was used to eliminate or minimize such interferences specially caused by palladium. Tellurium was measured by HG-ICP-AES and ICP-MS after separation of tellurium from SIMFUEL with cation exchange chromatography. The relative deviation between direct measurement and separation method was less than 6% based on the data by ICP-MS.

• Bulletin of the Korean Chemical Society
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• v.33 no.1
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• pp.177-182
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• 2012

A new composition of standardized Scutellariae Radix extract (HPO12) was developed for treatment of Alzheimer's disease. For the preclinical pharmacokinetic study of HPO12, a rapid, sensitive, and selective LCMS/MS method was developed and validated for the simultaneous determination of 4 bioactive compounds, baicalein, baicalin, wogonin, and wogonoside. After extraction with ethylacetate, chromatographic analysis was performed on a Thermo $C_{18}$ column ($150mm{\times}2.1mm$, $3{\mu}m$) with a mobile phase consisting of 0.1% formic acid (A) and 0.1% formic acid in 95% acetonitrile (B) by using gradient elution at a flow rate of $250{\mu}L/min$. Analytes introduced to a mass spectrometer were monitored by multiple reaction monitoring (MRM) in positive ion mode. Using $25{\mu}L$ of plasma sample, the method was validated over the following concentration ranges: 25-5000 ng/mL for baicalein, 20-40000 ng/mL for baicalin, 1-1000 ng/mL for wogonin, and 5-10000 ng/mL for wogonoside. The intra- and inter-day precision and accuracy of the quality control samples at the 4 concentrations showed $\leq$ 13.7% relative standard deviation (RSD) and 86.6-105.5% accuracy. The method was successfully applied to determine the concentrations of baicalein, baicalin, wogonin, and wogonoside in rat plasma after intraperitoneal and oral administrations of HPO12.

• YAKHAK HOEJI
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• v.42 no.5
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• pp.473-479
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• 1998

Lovastatin (LOVA), a fungal metabolite isolated from cultures of Aspergillus terreus, is a competitive HMG-CoA reductase inhibitor used for the treatment of primary hyper cholesterolemia, and has also been shown to suppress growth in a variety of non-glioma tumor cell lines. A sensitive reversed-phase high-perfonnance liquid chromatographic method with ultraviolet (UV) absorbance detection has been developed to quantitate LOVA in human plasma and urine samples using liquid-liquid extraction procedure. Baseline separation of LOVA and internal standard, simvastatin was achieved on a Novapak $C_{18}$ analytical column with a mobile phase containing 0.025M $NaH_2PO_4$: CAN (35:65, v/v%), adjusted pH to 4.5. The flow rate was set at 1.5ml/min, and the column effluent was monitored by a UV detection at 238nm. The limit of quantification was determined to be 0.5${\mu}$g/ml while extraction efficiency of LOVA ranged from 73.4-82.9% at LOVA concentrations of 0.5 to 10${\mu}$g/ml. Good linearity with correlation coefficients greater than 0.999 was obtained in the range of LOVA concentrations from 0.5 to 10${\mu}$g/ml. The accuracy and the precision were proven excellent with relative standard deviation (RSD, %) and relative error (RE, %) of less than 4.2 and 4.0, respectively. Intraday precision, evaluated at five LOVA concentrations (0.5, 1, 2, 5, 10${\mu}$g/ml) and expressed as RSD ranged from 0-1.82% while the interday precision at the same concentrations ranged from 0.7-10.5%. The analytical method described was then successfully employed for the determination of LOVA concentrations in plasma samples obtained during a phase II clinical trial using high doses of LOVA (30-40mg/kg/day). This method could be further utilized for the ongoing pharmacolkinetic studies and therapeutic drug monitoring of the high-dose LOVA therapy in adenocarcinoma patients.