• Journal of Food Hygiene and Safety
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• v.34 no.5
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• pp.413-420
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• 2019

In this study, a sample preparation method and a simultaneous determination method by ultra-high performance liquid chromatography coupled with tandem mass spectrometry for 9 isomers of chlorogenic acid and arbutin in fruits were developed. The samples were extracted using 90% methanol (pH 3.0), with the solutions being shaken and then sonicated for 10 min each. After centrifugation at 4,000 rpm for 10 min, the extraction was concentrated under a vacuum at $40^{\circ}C$ using a vacuum evaporator. The residue was dissolved in 5 mL of 5% methanol and filtered through a $0.45{\mu}m$ membrane before UHPLC-MS/MS analysis. The separations were performed on a C18 column with gradient elution of water (containing 0.1% formic acid) and methanol (containing 0.1% formic acid). The specificity, linearity, limit of detection, limit of quantification, accuracy, and precision of the proposed methods were also evaluated.

• Journal of Life Science
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• v.29 no.6
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• pp.653-661
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• 2019

The first small interfering RNA (siRNA) therapeutics have recently been approved by the Food and Drug Administration in the U.S., and the demand for a new RNA therapeutics bioanalysis method-which is essential for pharmacokinetics, including the absorption, distribution, metabolism, and excretion of siRNA therapeutics-is rapidly increasing. The stem-loop real-time qPCR (RT-qPCR) assay is a useful molecular technique for the identification and quantification of small RNA (e.g., micro RNA and siRNA) and can be applied for the bioanalysis of siRNA therapeutics. When the anti-HPV E6/E7 siRNA therapeutic was used in preclinical trials, the established stem-loop RT-qPCR assay was validated. The limit of detection was sensitive up to 10 fM and the lower limit of quantification up to 100 fM. In fact, the reliability of the established test method was further validated in three intra assays. Here, the correlation coefficient of $R^2$>0.99, the slope of -3.10 ~ -3.40, and the recovery rate within ${\pm}20%$ of the siRNA standard curve confirm its excellent robustness. Finally, the circulation profiles of siRNAs were demonstrated in rat serum, and the pharmacokinetic properties of the anti-HPV E6/E7 siRNA therapeutic were characterized using a stem-loop RT-qPCR assay. Therefore, the stemloop RT-qPCR assay enables accurate, precise, and sensitive siRNA duplex quantification and is suitable for the quantification of small RNA therapeutics using small volumes of biological samples.

• Korean Journal of Environmental Biology
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• v.40 no.3
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• pp.316-324
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• 2022

Ethyl formate (EF) is a potent fumigant replacing methyl bromide. The use of EF is limited to a quarantine process. Appling EF to agricultural field as a safe insecticide in greenhouse give us valuable benefits including less residual concern. In this regard, residual pattern after EF fumigation in greenhouse should be undertaken. In the previous study, we have established agricultural control concentration of EF to control pests in a greenhouse. EF was fumigated at 5 g m^-3 level for 2 h. The concentration of EF inside a greenhouse was analyzed to be 4.1-4.3 g m^-3 at 30 min after fumigation. To prepare an analytical method for residues in cucumber crops and soil in the greenhouse, the limit of detection(LOD) of the method was 100ng g^-1 and the limit of quantitation(LOQ) of this method was 300 ng g^-1. R² values of calibration curves for crops and soil were 0.991-0.997. In samples collected immediately after ventilation, EF concentration was determined to be below LOQ level. In addition, EF level was below LOQ in samples collected at 3 h after ventilation except that leaf samples of melon during the flowering period showed a level of 1,068.9 ng g^-1. Taken together, these results indicate that EF used in quarantine can be applied to agricultural fields without residual issue as an effective fumigant for insect pest control.

• Journal of the Korean Chemical Society
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• v.37 no.5
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• pp.513-522
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• 1993

The purpose of this study is to optimize the selectivity of mobile phase solvents for separation of 25 phenols in reversed phase liquid chromatography and to accomplish the simultaneous preconcentration and separation of trace phenols from water samples. Phenols used in this study were classified into three groups, chloro-, methyl-, and nitrophenols. Quaternary solvent mobile phases were employed to improve the selectivity. Overlapping resolution maps(ORM) as a statistical simplex techniques was used to predict the optimum solvent system. Additional criterion such as pH and temperature were also investigated. In order to improve the resolution and decrease the analysis time, isoselective multisolvent gradient elution system was employed with ORM-Prism method. The simultaneous preconcentration and separation of trace phenols from water samples were performed by using XAD-2/Dowex 1-X8 tandem column. When the extraction efficiency was evaluated by sampling up to 1 L of distilled water, recovery of the phenols, except phenol, was above 90% and the limit of detection of the phenols was 5 ppb. The XAD-2/Dowex 1-X8 method was superior to C18 cartridge in terms of recovery and selectivity.

• Journal of Korean Society of Occupational and Environmental Hygiene
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• v.21 no.3
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• pp.139-145
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• 2011

Objectives: This investigation is purposed to evaluate the airborne asbestos concentrations in the public buildings having asbestos containing materials(ACMs) in Seoul. Methods: The Seoul Metropolitan Government carried out an asbestos survey to the city-owned public buildings to identify the level of risk exposure, classified into low, moderate and high risk. To evaluate the airborne concentration of asbestos, 11 sampling sites in ten buildings based on the survey were selected. The air samples from the eleven sites were analyzed by Phase Contrast Microscopy(PCM) and Transmission Electron Microscopy (TEM), and compared the analytical results from the both. Results: 1. The airborne fiber concentrations by PCM were less than the detection limit($7f/mm^2$) in 9(82%) out of 11 sampling sites. The highest concentration was 0.0043 f/cc, but it was below the guideline value for indoor air quality(0.01 f/cc), proposed by the Ministry of Environment, Korea. 2. In two sampling sites, having moderate risk level, the chrysotile was identified and showed it's concentrations of 0.0102 s/cc and 0.0058 s/cc, less than $5{\mu}m$ lengths. 3. The ACMs identified in the two sampling sites were a packing material(65% of chrysotile) in mechanical area and a thermal system insulation(5% of chrysotile) in a boiler room. Having more possibility of asbestos emission in the mechanical area, it would be required to set up and carry out the asbestos management plan. Conclusions: Based on the result of this study, the airborne asbestos concentrations in the public buildings with ACMs were generally lower than the guideline value for indoor air quality. There are widespread concerns about the possible health risk resulting from the presence of airborne asbestos fibers in the public buildings. Most of the previous studies about airborne asbestos analysis in Korea were performed based on PCM method that asbestos and non-asbestos fibers are counted together. In the public and commercial buildings, having ACMs, it is suggested that the asbestos be analyzed by TEM method to identify asbestos due to concerns about asbestos exposure to workers and unspecified people.

• Analytical Science and Technology
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• v.11 no.5
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• pp.409-412
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• 1998

The analytical method to determine europium(III) ion in aqueous solution by fluorescence spectroscopy based upon the conformational change of calmodulin in the presence of the analyte has been studied. The fiber optic chemical sensor used in this study was constructed by entrapping a fluorescein-labeled calmodulin solution, EGTA, buffer solution at the common end of a bifurcated fiber optic bundle by means of a dialysis membrane. The calibration curve to determine europium(III) ion was obtained when concentration of calmodulin, concentration of EGTA, Tris-HCl buffer solution, pH, excitation wavelength and fluorescence wavelength were $5.0{\times}10^{-5}M$, 0.50 mM, 5.0 mM, 7.0, 495 nm and 520 nm, respectively. The detection limit was $1.0{\times}10^{-11}M$ and the working range of the calibration curve for the sensor was $1.0{\times}10^{-11}M{\sim}1.0{\times}10^{-9}M$. The response time was 15 minutes. For the determination of europium(III) ion by the present method, $Na^+$ and $K^+$ ions did not interfere but $Ca^{2+}$ ion seriously interfered.

• Journal of Environmental Science International
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• v.15 no.1
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• pp.85-94
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• 2006

The simultaneous analysis of multi-residual pesticides was developed using a gas chromatography (GC) method. In this study, a simple and reliable methodology was improved to detect 154 kinds of pesticides in sinseng extract sample by using a liquid-liquid extraction procedure, open column chromagraphy and chromatographic analysis by CC electron capture detector (ECD) and GC nitrogen-phosphorus detector (NPD). The 154 kinds of pesticides were classified in 4 groups according to the chemical structure. The extraction of pesticides was experimented with $70\%$ acetone and dichloromethane/petroleum ether in order, and cleaned up via open column chromatography $(3\times30cm)$ packed with florisil $(30g,\;130^{\circ}C,\;12hrs)$. The final extract was concentrated in a rotator evaporator at $40^{\circ}C$ until dryness. Then the residue was redissolved to 2ml with acetone, and analyzed by GC-ECD and GC-NPD. The applied concentration of pesticides was over $1\~10{\mu}g/ml$. The recovery tests were ranged from $70.7\%$ to $115.2\%$ with standard deviations between 0.3 and $5.7\%$ of the standard spiked to the ginseng extract sample (Group $I\~IV$). The limit of detection (LOD) ranged from 0.001 to $0.099{\mu}g/ml$ (Group $I\~IV$). The 9 kinds of pesticides were not detected. The developed method was applied satisfactory to the determination of the 154 kinds of pesticides in the ginseng extract with good reproducibility and accuracy.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.40 no.1
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• pp.37-44
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• 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 the Korean Society of Food Science and Nutrition
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• v.39 no.8
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• pp.1231-1235
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• 2010

The method for residue analysis of four sulfonylurea pesticides, rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl and chlorimuron-ethyl was examined and analyzed by HPLC with ODS column ($250\;mm{\times}4.6\;mm$, $5\;{\mu}m$ diameter particle size) which was maintained at $35^{\circ}C$. Mobile phase consisted of solvent A (20 mM $KH_2PO_4$, pH 2.5) and solvent B (acetonitrile). Isocratic elution of the column with 45% solvent A and 55% solvent B at a flow rate of 1 mL/min resulted in retention times of 5.92, 6.54, 9.28, and 14.35 min for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. All injection volumes were $20\;{\mu}L$. The limit of quantitation was 0.02, 0.01, 0.001, and 0.004 mg/kg for rimsulfuron, ethametsulfuron-methyl, tribenuron-methyl, and chlorimuron-ethyl, respectively. Recovery rate test was performed with three farm products, rice, apple and soybean. Four sulfonylurea pesticides were spiked at concentrations of 0.05, 0.1 and 0.5 mg/kg. The recovery rates were ranged from 86.12% to 116.26% and the standard deviations of all experiments were within 10%.

• Biomedical Science Letters
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• v.3 no.1
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• pp.29-35
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• 1997

Cardiovascular disease has been the leading cause of death among patients with chronic renal failure. Many reports have been described that homocysteine is one of the independent risk factor to the occulsive vascular disease. In this study, HPLC/FLD (high performance liquid chromatography-fluorescence detector) technique was used to measure homocysteine level in patients with chronic renal failure and normal control group. The detection limit and recovery of total plasma homocysteine using HPLC/FLD were 98.6$\pm$5.8% and 0.2 nmol/ml, respectively. The linearity of this method was established in concentration range of 2~50 nmol/ml (correlation coefficient=0.9997). The concentrations of total plasma homocysteine were 6.81$\pm$1.54 nmol/ml and 27.28$\pm$14.94 nmol/ml in normal control (n=20) and patient group (n=90), respectively (p<0.05). In this study, the HPLC/FLD method showed high sensitivity and reproducibility for a routine clinical laboratory testing. Moreover determination of homocysteine level in plasma might be useful for a biochemical marker for predicting the cardiovascular diseases and for monitoring of therapeutic effect of lowering homocysteine in patients with chronic renal failure.