• Natural Product Sciences
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• v.25 no.1
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• pp.49-58
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• 2019

Eleven steroid hormones (SHs: androstene-3,17-dione, estrone, ${\beta}$-estradiol, ${\alpha}$-estradiol, testosterone, dehydroepiandrosterone, $17{\acute{a}}$-hydroxyprogesterone, medroxyprogesterone, megestrol acetate, progesterone, and androsterone) were detected from New Zealand deer (Cervus elaphus var. scoticus) velvet antler (NZA, 鹿茸 ). A method for the quantification of eleven SHs was established by using ultraperformance liquid chromatography (UPLC)-MS/MS. The linearities ($R^2$ > 0.991), limits of quantification (LOQ values, 0.3 ng/mL to 23.1 ng/mL), intraday and interday precisions (relative standard deviation: RSD < 2.43%), and recovery rates (97.3% to 104.6%) for all eleven SHs were determined. In addition, a method for the quantification of three 7-oxycholesterols (7-O-CSs: 7-ketocholesterol, $7{\alpha}$-hydroxycholesterol, and $7{\beta}$-hydroxycholesterol) in the NZA was established by using an HPLC-photodiode array (PDA) method. The linearities ($R^2$ > 0.999), LOQ values (30 ng/mL to 350 ng/mL), intraday and interday precisions (RSD < 1.93%), and recovery rates (97.2% to 103.5%) for the three 7-O-CSs were determined. These quantitative methods are accurate, precise, and reproducible. As a result, it is suggested that the five steroid compounds of androstene-3,17-dione, androsterone, 7-ketocholesterol, $7{\alpha}$-hydroxycholesterol, and $7{\beta}$-hydroxycholesterol could be marker steroids of NZA. These methods can be applied to quantify or standardize the marker steroids present in NZA.

• Journal of the Korean Society of Radiology
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• v.15 no.1
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• pp.79-83
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• 2021

In radiation therapy, electron beam is often used in the treatment of superficial lesion. Accurate measurements are required because electron beam interacts with them in the beam path and affects dose measurements. However, no research has been conducted on electron beam quality assurance. in this study, PbO-based dosimeter was fabricated as a basic study for electron beam quality assurance. Thus, the reproducibility and linearity of the energy of 6, 9, and 12 MeV were analyzed to evaluate measurement accuracy and precision. Reproducibility measurements show RSD value of 1.024%, 1.019% and 0.890%, respectively, at 6, 9, and 12 MeV. linearity measurements show 0.9999 R2 at 6, 9, and 12 MeV altogether. Both evaluations show that the PbO dosimeter has very good measurement accuracy and precision with excellent results.

• Natural Product Sciences
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• v.28 no.4
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• pp.187-193
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• 2022

Lysimachia christinae Hance was commonly used in Oriental medicine for treating the hepatitis virus, cholecystitis and cholagogic efficiency. According to the previous study, it possesses high antioxidant and anti-inflammatory activity. Simultaneous determination analytical method of isolated eight compounds, cynaroside (1), 2-(3,4-dimethoxyphenyl) ethyl O-α-L-arabinopyranosyl-(1→2)-O-[6-deoxy-α-L-mannopyranosyl-(1→3)] β-D-glucopyranoside (2), stearylester ricinoleic acid (3), (E)-4-(3,4-dimethoxyphenyl) but-3-en-1-yl palmitate (4), 2-hydroxy-24-methoxy-4-tetracosenoic acid (5), 2-hydroxy-24-propoxy-4-tetracosenoic acid (6), β-sitosterol (7), and androst-16-ene-3,6-diol (8) were established by using HPLC-DAD. This HPLC analysis was detected on a Dionex C18 column (5 ㎛, 120 Å, 4.6 mm × 150 mm) at 25℃. The mobile phase consisted of 0.1% trifluoroacetic acid and acetonitrile at a flow rate of 1 mL/min. Validation of the method was assessed by linearity, precision and accuracy test. Calibration curve was good at r² > 0.9998. Limits of detection (LOD) ranged from 0.19 to 8.18 g/ml and Limits of quantification (LOQ) ranged from 0.19 to 24.80 g/ml. The relative standard deviations (RSD) values of precision test, intra- and inter- day, were less than 0.99% and 1.0%. The accuracy test results ranged from 98.81% to 106.49% and RSD values were less than 0.95%. These results showed that the HPLC-DAD method was very reliable and accurate for the quantity analysis of eight compounds in L. christinae extract for quality control.

• Analytical Science and Technology
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• v.21 no.5
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• pp.424-431
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• 2008

Streptomycin, which is one of aminoglycoside antibiotics, has been widely used in the rearing of food-producing animals to prevent and treat diseases in cattle, pigs and poultry. Although not licensed in South Korea, streptomycin has also been used for the treatment of bacterial honeybee disease, such as European foulbrood in Third World countries. A reliable and effective method using liquid chromatography-tandem mass spectrometry (LC-MS/MS) was developed for the determination of streptomycin in honey. A established method was optimized the clean-up and extraction procedure for the trace determination, good precision and accuracy. And the chromatographic and tandem mass spectrometric parameters were also optimized. The precision (RSD) and accuracy (bias) in the concentration range of 5.0~50.0 ug/kg were 5.5~14% and -10.0~8.0%, respectively. Limit of detection was 0.75 ug/kg and recovery of streptomycin spiked at level of 10 ug/kg in honey was 74%. The established and validated method was applied to determine streptomycin in honey which was on the market.

• Analytical Science and Technology
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• v.21 no.6
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• pp.502-509
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• 2008

An ID LC/MS (isotope dilution liquid chromatography/mass spectrometry) was used as a primary method for the quantitative analysis of cholesterol in human serum. The separation of cholesterol was carried out by Thermo ODS hypersil $C^{18}$ column. The mobile phase was 100% methanol, and flow rate was $0.3m{\ell}/min$. Cholesterol and cholesterol-$3,4-13C_2$ were monitored at m/z 369.4 and 371.3, which correspond to $[M-H_2O+H]^+$ respectively. In order to verify the measurement method, NIST SRM 909b was analyzed. The results agreed well with certified values within uncertainty. The four kinds of serum certified reference material were prepared and certified. The repeatabilities of measurement were ranged from 0.1 to 0.8% (RSD), which were relatively good. The reproducibility between independent measurement run was below 0.24% (RSD). The expanded uncertainty was about 1.43% within the 95% confidence interval.

• Journal of the Korean Society of Radiology
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• v.11 no.7
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• pp.671-677
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• 2017

In this study, scattering factors affecting the quality of medical images were quantitatively analyzed and investigated. MCNPX simulation was conducted by using ANSI phantom, made of tissue equivalent materials, to calculate the scattering ratio occurred by the increase of the object thickness. Then, the result of the simulation was compared with the result of actual radiation measurement. In addition, we evaluated the image quality by the RMS evaluation, RSD and NPS analysis using X-ray images acquired with increasing object thickness. Furthermore, the scattering ratio was analyzed by increasing the thickness of acrylic phantom on chest phantom. The result showed that the scattering ratio was increased to 57.2%, 62.4%, and 66.8% from 48.9%, respectively, when the acrylic phantom thickness was increased by 1 inch from 6.1 inches. The results of MCNPX simulation and the actual measured scattering dose showed similar results. Also, as a result of RMS measurement from acquired x-ray images, the standard deviation decreased as the object thickness increased. However, in the RSD analysis considering the average incident dose, the results were increased from 0.028 to 0.039, 0.051, 0.062 as the acrylic phantom thickness was increased from 6.1 inches to 7.1 inch, 8.1 inch, and 9.1 inch, respectively. It can be seen that the increase of the scattering effect due to the increase of the object thickness reduces the SNR. Also, the NPS results obtained by measuring scattered radiation incident on the detector resulted in the increase of the noise as the object thickness increased.

• Analytical Science and Technology
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• v.24 no.3
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• pp.193-199
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• 2011

The purpose of this experiment is to evaluate the stability of products according to the storage methods, the period of use, and the diurnal variations through the short term stability experiment of recombinunt protein A (rProtein A) produced in AP Tech Co. That is, we investigated how long the stability of the products would last, when we used the samples frozen at $-20^{\circ}C$, which is one of the storage conditions of the produced rProtein A and then kept them refrigerated at $4^{\circ}C$. The experiment was conducted for 8 weeks and 6 experiment points were established. The experiment was done by thawing the samples frozen at $-20^{\circ}C$ at room temperature, and then refrigerating them at $4^{\circ}C$. In addition, experiments for endotoxin, bioburden, HPLC purity, and concentration were conducted. As a result of the experiment, 0.5 EU/mg endotoxin was detected both at the beginning and at the 8th week and bioburden was not analyzed. In the case of purity, it showed 99.23~99.90% at 210 nm (RSD% 0.23%) and 100% at 280 nm, which meant the change into other materials didn't happen and there was no material degradation characteristics. Finally, we also found the fact that the concentration stayed stable at 55.15 mg/mL (RSD% 0.55%) both at the beginning and at the end. From the experiment results, we were able to conclude that the stability at the condition to store rProtein A at 4 oC for 8 weeks was procured without producing microorganisms or having material degradation characteristics.

• The Korean Journal of Pesticide Science
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• v.16 no.2
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• pp.121-130
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• 2012

In analyzing pesticide residue, LLE (liquid liquid extraction) is generally applied as one of the existing methods, but needed quite a lot of organic solvents and analytical apparatuses for the sample pre-treatment. In addition to its long analysis time and complex analytical processes, it is required to develop a more rapid and efficient method at present. In order to establish an economic and simple pesticide residue analytical method, this study carried out a comparative experiment on the existing analytical method with a new sample pre-treatment method named QuEChERS (quick, easy, cheap, effective, rugged and safe), which extracts and refines pesticide components by directly adding solid powder into the sample. Both the two analytical methods showed favorable values of correlation coefficient ($R^2$ > 0.99) of calibration curves. In terms of the detection limit (identification limit), imidacloprid showed 0.02 mg/kg, while the rest of pesticides showed a level around 0.05 mg/kg. The results of this experiment revealed that the recovery of LLE was 92.8-100.9% and the RSD was below 2.5%. On the other hand, the recovery of QuEChERS was 92.2-101.6% and RSD was below 1.9%. As a result of comparing the amount of pesticide residue by the time between the two analytical methods by using Paired t-Test, there was no significant difference between the two analytical methods as the p-value ranged from 0.3148-0.9890. Considering the results of the two methods, the QuEChERS method had similar recovery, compared to the analytical method using the existing LLE, and the analytical time was shortened by about one fourth of that of the existing method. Moreover, since it excludes the use of harmful organic solvents like dichloromethane during the process of extraction, thus leading to protecting experimenters health and remarkably reducing the amount of disused solvents, it is judged as an echo-friendly and economic analytical method.

• The Korean Journal of Pesticide Science
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• v.15 no.4
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• pp.401-416
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• 2011

The recent trend for pesticide residue analysis in food involves fast cleanup and use of mass spectrometry to achieve quantitative and qualitative analysis at the same time. Recently, the QuEChERS (quick, easy, cheap, effective, rugged and safe) multi-reside method has received much attention as a fast extraction and cleanup method of pesticide residue analysis. Therefore, multi-residue analysis of 236 pesticides was tested with the QuEChERS method by concurrent use of PTV-GC/TOFMS (gas chromatography/ time-of-flight mass spectrometry with programmable temperature vaporizer). PTV condition was optimized and when the method was applied to apples, pesticide recovery rates (spiked at 400 ng/g) ranged from 80% to 120%, and RSD values were under 10% for most compounds. The results showed that the QuEChERS sample preparation and PTV-GC/TOFMS analysis can be applied to multi-residue analysis of pesticides in fruits and vegetables.

• Journal of the Korean Society of Food Science and Nutrition
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• v.44 no.1
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• pp.85-88
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• 2015

This study attempted to establish an HPLC analysis method for determination of marker compounds as a part of material standardization for the development of health functional food materials from Perilla frutescens Britton var. acuta Kudo. The quantitative determination method of rosmarinic acid as a marker compound of P. frutescens Britton var. acuta Kudo extract (PFE) was optimized by HPLC analysis using a C18 column ($4.6{\times}150mm$, $5{\mu}m$) with 0.1% acetic acid as the elution gradient and methanol as the mobile phase at a flow rate of 1 mL/min and detection wavelength of 280 nm. The HPLC/UV method was applied successfully to quantification of the marker compound in PFE 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 0.9995, and the limit of detection and limit of quantitation were $0.36{\mu}g/mL$ and $1.2{\mu}g/mL$, respectively. Relative standard deviation (RSD) values of data from intra- and inter-day precision were less than 3.21% and 1.43%, respectively. Recovery rate test at rosmarinic acid concentrations of 12.5, 25 and $50{\mu}g/mL$ scored between 97.04~98.98% with RSD values from 0.25~1.97%. These results indicate that the established HPLC method is very useful for the determination of marker compound in PFE to develop a health functional material.