• The Transactions of The Korean Institute of Electrical Engineers
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• v.67 no.12
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• pp.1626-1632
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• 2018

In this paper, we describe the fabrication and characterization of a hydrogen peroxide ($H_2O_2$) sensor based on palladium and copper (PdCu) electroplated laser induced graphene (LIG) electrodes. $CO_2$ laser was used to form LIG electrodes on a PI film. This fabrication method allows simple control of the LIG electrode size and shape. The PdCu was electrochemically deposited on the LIG electrodes to improve the electrocatalytic reaction with $H_2O_2$. The electrochemical performance of this sensor was evaluated in terms of selectivity, sensitivity, and linearity. The physical characterization of this sensor was conducted using scanning electron microscopy (SEM) and energy-dispersive X-ray spectroscopy (EDS), which confirmed that PdCu was formed on the laser induced graphene electrode. In order to increase the sensor sensitivity, the Pd:Cu ratio of the electroplated PdCu was varied to five different values and the condition of highest amperometric current at an identical of $H_2O_2$ concentration was chosen among them. The resulting amperometric current was highest when the ratio of Pd:Cu was 7:3 and this Pd;Cu ratio was employed in the sensor fabrication. The fabricated PdCu/LIG electrode based $H_2O_2$ sensor exhibited a sensitivity of $139.4{\mu}A/mM{\cdot}cm^2$, a broad linear range between 0 mM and 16 mM of $H_2O_2$ concentrations at applied potential of -0.15 V, and high reproducibility (RSD = 2.6%). The selectivity of the fabricated sensors was also evaluated by applying ascorbic acid, glucose, and lactose separately onto the sensor in order to see if the sensor ourput is affected by one of them and the sensor output was not affected. In conclusion, the proposed PdCu/LIG electrode based $H_2O_2$ sensor seems to be suitable $H_2O_2$ sensor in various applications.

• Journal of Food Hygiene and Safety
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• v.34 no.1
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• pp.52-57
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• 2019

Method development and validation of decursin for the standardization of Angelica gigas Nakai as a functional ingredient and health food were accomplished. The quantitative determination method of decursin as a marker compound of aerial parts of Angelica gigas Nakai extract (AAGE) was optimized by HPLC analysis using a C18 column ($3{\times}150mm$, $3{\mu}m$) with 0.1% TFA in water and acetonitrile as the mobile phase at a flow rate of 0.5 mL/min and detection wavelength of 330 nm. The HPLC/PDA method was applied successfully to quantification of the marker compound in AAGE after validation of the method with linearity, accuracy, and precision. The method showed high linearity in the calibration curve at a coefficient of correlation ($R^2$) of 0.9994 and the limit of detection and limit of quantitation were $0.011{\mu}g/mL$ and $0.033{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 1.10% and 1.13%, respectively. Recovery of decursin at 0.5, 1, 5 and $10{\mu}g/mL$ were 92.38 ~ 104.11%. These results suggest that the developed HPLC method is very useful for the determination of marker compound in AAGE to develop a health functional material.

• Analytical Science and Technology
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• v.32 no.1
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• pp.24-34
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• 2019

The safety of food is occasionally questionable, as there have been some reports of products contaminated with illegal adulterants. In this study, the presence of 16 sedative-hypnotics and sleep inducers in dietary supplements was determined by ultra-high-performance liquid chromatography with UV detection (UPLC-UV) and quadruple Orbitrap mass spectrometry (Q-Orbitrap-MS). The UPLC method was validated, providing a linearity (R2) of more than 0.999, and LODs and LOQs that ranged from 0.2 to 0.5 and 0.6 to $1.5{\mu}g\;mL^{-1}$, respectively. The repeatabilities were 0.2-8.4 % (intra-day) and 0.3-4.5 % (inter-day), and the accuracies were 89.0-117.0 % (intra-day) and 87.8-111.9 % (inter-day). The mean recoveries of the spiked samples ranged from 98.7 to 107.3 %. The relative standard deviation (%RSD) of the stability was less than 2.4 %. Using the developed method, one sedative-hypnotic compound, phenobarbital, was detected in one of the nineteen samples tested. In addition, the major characteristic fragment ions of each target compound were confirmed using Q-Orbitrap-MS for higher accuracy. Monitoring the presence of these 16 sedative-hypnotics and sleep inducers in dietary supplements should be pursued in the interest of human health, and the results of this study confirmed that the developed method has value for this application.

• Korean Journal of Food Science and Technology
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• v.51 no.4
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• pp.301-308
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• 2019

The antioxidant properties of Eriobotrya japonica leaf extract were investigated using DPPH and ABTS radical scavenging assay. The 80% ethanol extract of leaves ($IC_{50}$ values for DPPH and ABTS were 13.9 and $10.9{\mu}g/mL$, respectively) and young leaves ($IC_{50}$ values for DPPH and ABTS were 20.7 and $17.3{\mu}g/mL$, respectively) showed high radical scavenging activity. Additionally, the quantitative method for estimation of ellagic acid and chlorogenic acid from E. japonica leaves was optimized by HPLC/DAD. This method showed high linearity of the calibration curve with a coefficient of correlation ($R^2$) equal to 0.999. The LOD values for ellagic acid and chlorogenic acid were 2.35 and $0.73{\mu}g/mL$, respectively, whereas LOQ values were 7.13 and $2.22{\mu}g/mL$, respectively. Recovery of the two compounds was 99.7-108.0% with RSD values less than 5.31%. These results suggest that 80% ethanol extract of E. japonica leaves could serve as a potential source of natural antioxidant for us in various industrial applications.

• Analytical Science and Technology
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• v.32 no.2
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• pp.35-47
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• 2019

In this study, high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) was employed to detect 26 antidiabetic compounds in adulterated dietary supplements using a simple, selective method. The work presented herein may help prevent incidents related to food adulteration and restrict the illegal food market. The best separation was obtained on a Shiseido Capcell Pak(R) C18 MG-II ($2.0mm{\times}100mm$, $3{\mu}m$), which improved the peak shape and MS detection sensitivity of the target compounds. A gradient elution system composed of 0.1 % (v/v) formic acid in distilled water and methanol at a flow rate of 0.3 mL/min for 18 min was utilized. A triple quadrupole mass spectrometer with an electrospray ionization source operated in the positive or negative mode was employed as the detector. The developed method was validated as follows: specificity was confirmed in the multiple reaction monitoring mode using the precursor and product ion pairs. For solid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL, and for liquid samples, LOD ranged from 0.16 to 20.00 ng/mL and LOQ ranged from 0.50 to 60.00 ng/mL. Satisfactory linearity was obtained from calibration curves, with $R^2$ > 0.99. Both intra and inter-day precision were less than 13.19 %. Accuracies ranged from 80.69 to 118.81 % (intra/inter-day), with a stability of less than 14.88 %. Mean recovery was found to be 80.6-119.0 % and less than 13.4 % RSD. Using the validated method, glibenclamide and pioglitazone were simultaneously determined in one capsule at concentrations of 1.52 and 0.53 mg (per capsule), respectively.

• Journal of Food Hygiene and Safety
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• v.36 no.1
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• pp.34-41
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• 2021

The purpose of this research is to improve analysis methods of determining the contents of fatty acids in infant formulas and follow-up formulas. A gas chromatography (GC) method was performed on a GC system coupled to flame ionization detector, with a fused silica capillary column (SP2560, 100 m×0.25 mm, 0.20 ㎛). The method was validated using standard reference material (SRM, NIST 1849a). Performance parameters for method validation such as specificity, linearity, limits of detection (LOD) and quantification (LOQ), accuracy and precision were examined. The linearity of standard solution with correlation coefficient was higher than 0.999 in the range of 0.1-5 mg/mL. The LOD and LOQ were 0.01-0.06 mg/mL and 0.03-0.2 mg/mL, respectively. The recovery using standard reference material was confirmed and the precision was found to be between 0.8% and 2.9% relative standard deviation (RSD). Optimized methods were applied in sample analysis to verify the reliability. All the tested products had acceptable contents of fatty acids compared with component specification for nutrition labeling. The result of this research will provide efficient experimental information and strengthen the management of nutrients in infant formula and follow-up formula.

• Journal of Korean Society on Water Environment
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• v.37 no.6
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• pp.510-519
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• 2021

Volatile Organic Compounds (VOCs) in sediments, which can cause human health problems, have been monitored in Korea since 2014. Measured VOC concentrations can be affected by matrix type and the volatility of target substances. In this study, (1) VOCs volatility and the influence of matrix interference were confirmed, and (2) internal standards (IS) method was applied to improve analytical method. For these purposes, method detection limit (MDL), calibration linearity, precision and accuracy of VOCs were compared in various matrices using the IS. Some of VOCs in sediments showed different peak areas and reduced rates compared to water matrix. It was suggested that adsorption properties of sediments hindered the migration to vapor during heat pretreatment in headspace method. A calibration curve was created in clean sand. Recovery rates for the calibration curve method and IS applying method were 64.1~83.1% and 99.1~119.3%, respectively. Relative standard deviations ranged from 11.1% to 21.6% for the calibration curve method and those for IS ranged 4.7% to 13.7%. In case of real sediment, calibration curve and 1,2-Dichlorobenzene-d4 (ODCB) among IS were not suitable. The average recovery rate of Fluorobenzene (FBZ) increased by 56.4% and Relative Standard Deviation (RSD) by 4.7%. However, the recovery rate was increased in the samples with large values of igniting intensity. This study confirmed that influence of the matrix of VOCs in sediment, and addition of IS materials improved precision and accuracy. Although IS corrects volatilization and adsorption, it is recommended that more than two types of IS should be added rather than single.

• Korean Journal of Environmental Agriculture
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• v.42 no.3
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• pp.203-210
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• 2023

Ferimzone Z is a fungicide for effectively controlling rice blast. Under light irradiation conditions, it undergoes a rapid conversion to its E-stereoisomer. Given the importance of isomers in risk assessments of residues in crops, an analytical method was developed for individual isomer quantification. A comparative analysis performed using two columns in HPLC-MS/MS demonstrated that the isomers were successfully separated using the Cadenza column. For the brown rice sample preparation, 5 g of the homogenized sample was saturated with 7 mL of water. The sample was then extracted with a 10 mL mixed solvent of acetonitrile and ethyl acetate (1:1, v/v) that contained 0.1% formic acid, and it was subsequently partitioned with magnesium sulfate and sodium chloride. The upper layer was purified using dSPE containing C₁₈ and PSA sorbents. The established method was subjected to method validation, and it showed recovery rates of 90.6-98.8% (RSD ≤ 3.9%) at concentrations of 0.01, 0.1, 2 mg/kg, with a soft matrix effect (%ME) ranging from -3.1% to +6.5%. This method can be employed in monitoring studies of brown rice to determine the conversion ratio from the Z isomers to the E isomers.

• Analytical Science and Technology
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• v.22 no.5
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• pp.386-394
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• 2009

Formaldehyde is used in lether manufacture, a dry plate and an explosive. It is by-product of ozonizing process in filtration plant. The effects of exposure are eye pruritus, tickle, runing nose, blocking nasal passages and headache. It also makes a dried throat and causes inflammation. It is classified as B1 group for inhalation by US. EPA, which can cause cancer in human. For analysis of formaldehyde, formaldehydes-DNPH derivative was extracted with solid cartridge and was analyzed by High Performance Liquid Chromatography/Diode Array Detector (HPLC/DAD). The detection limit was $3{\mu}g/L$ and the recoveries were 72.3~109.1% (RSD 2.9~11.5%). Water samples were collected in four Korean rivers, four times per year seasonally for 10 years from 1998 to 2007. The monitoring results were 48.8% (630/1291), $5.15{\sim}101.9{\mu}g/L$ in purified water. Because of non-carcinogen in drinking water, hazard index is calculated with RfD. Results of excess cnacer risk was below 1 and was considered as safe value.

• Advances in nano research
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• v.13 no.5
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• pp.417-426
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• 2022

Bisphenol A (BPA) is one of the chemicals used in monomer epoxy resins and polycarbonate plastics. The surface-enhanced Raman spectroscopy (SERS) method is precise for identifying biological materials and chemicals at considerably low concentrations. In the present article, the substrates coated with gold nanoparticles have been studied to identify BPA and control the diseases caused by this chemical. Gold nanoparticles were made by a simple chemical method and by applying gold salt and trisodium citrate dihydrate reductant and were coated on glass substrates by a spin-coat approach. Finally, using these SERS substrates as plasmonic sensors and Raman spectroscopy, the Raman signal enhancement of molecular vibrations of BPA was investigated. Then, the molecular vibrations of BPA in some consumer goods were identified by applying SERS substrates as plasmonic sensors and Raman spectroscopy. The fabricated gold nanoparticles are spherical and quasi-spherical nanoparticles that confirm the formation of gold nanoparticles by observing the plasmon resonance peak at 517 nm. Active SERS substrates have been coated with nanoparticles, which improve the Raman signal. The enhancement of the Raman signal is due to the resonance of the surface plasmons of the nanoparticles. Active SERS substrates, gold nanoparticles deposited on a glass substrate, were fabricated for the detection of BPA; a detection limit of 10-9 M and a relative standard deviation (RSD) equal to 4.17% were obtained for ten repeated measurements in the concentration of 10-9 M. Hence, the Raman results indicate that the active SERS substrates, gold nanoparticles for the detection of BPA along with the developed methods, show promising results for SERS-based studies and can lead to the development of microsensors. In Raman spectroscopy, SERS active substrate coated with gold nanoparticles are of interest, which is larger than gold particles due to the resonance of the surface plasmons of gold nanoparticles and the scattering of light from gold particles since the Raman signal amplifies the molecular vibrations of BPA. By decreasing the concentration of BPA deposited on the active SERS substrates, the Raman signal is also weakened due to the reduction of molecular vibrations. By increasing the surface roughness of the active SERS substrates, the Raman signal can be enhanced due to increased light scattering from rough centers, which are the same as the larger particles created throughout the deposition by the spin-coat method, and as a result, they enhance the signal by increasing the scattering of light. Then, the molecular vibrations of BPA were identified in some consumer goods by SERS substrates as plasmonic sensors and Raman spectroscopy.