• Journal of Digital Convergence
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• v.10 no.6
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• pp.331-339
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• 2012

The easy and simple simultaneous analytical method of preservatives (BA, SA, DHA, MP, EP, IPP, PP, IBP and BP) was studied by more easily changing from method used in food and drug using HPLC with scherzo SM-C18 column. All presevatives were seperated successfully in mobile phase of 50 mM ammonium formate : 0.1% phosphoric acid (50:50 v/v%) and 50 mM ammonium formate : acetonitrile (30 : 70). Retention time of BA, SA, DHA, MP, EP, IPP, PP, IBP and BP was 7.74, 9.08, 12.57, 13.83, 21.62, 27.29, 28.20, 33.20 and 33.68 min, respectively. The calibration curves of BA, SA, DHA, MP, EP, IPP, PP, IBP and BP were linear over the concentration range of 5~80 ${\mu}g/mL$ with correlation coefficient of above 0.999. The limit of detection (LOD) and limit of quantitation (LOQ) of BA, SA, DHA, MP, EP, IPP, PP, IBP and BP were 0.52 and 1.58, 1.09 and 3.29, 1.00 and 3.03, 1.36 and 4.13, 1.26 and 3.83, 1.02 and 3.08, 1.11 and 3.37, 0.82 and 2.48, 0.85 and 2.59 ${\mu}g/mL$, respectively. The coefficients of variation for intra- and inter-day assay were 0.12~2.68 and 0.18~2.66%, respectively. The developed method showed good intra- and inter-day precision and accuracy. The preservatives used in mouthwashes were BA, MP and PP and were detected in 24 samples(86%) except for 4 samples and not showed significant difference in using dose of adult and children. In conclusion, the developed method can be useful for simultaneous analysis of preservatives in mouthwashes and these results suggest that could be applied to fundamental study and guideline on content of preservatives in mouthwashes.

• Fisheries and Aquatic Sciences
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• v.23 no.3
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• pp.9.1-9.6
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• 2020

Background: Fucosterol is a compound commonly found in algae that has various biological activities. The purpose of this study was to develop a high-performance liquid chromatography (HPLC) validation method for fucosterol and to compare the fucosterol contents of 11 algal species from Ulleungdo, Korea. Method: In this study, we successfully isolated and identified fucosterol from a 70% EtOH extract of Sargassum miyabei, and subsequently conducted specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, and precision analyses for development of an HPLC validation method. Fucosterol contents were compared using the established HPLC validation conditions. Results: We successfully isolated fucosterol from a 70% EtOH extract of S. miyabei and identified it based on spectroscopic analysis. On the basis of HPLC validation using the fucosterol isolated from S. miyabei, we confirmed specificity (8.5 min), linearity (R² = 0.9998), LOD (3.20 ㎍ mL^-1), LOQ (9.77 ㎍ mL^-1), accuracy (intra-day and inter-day variation, 90-110%), and precision (RSD, 1.07%). Fucosterol contents in the 11 assessed algal species ranged from 0.22 to 81.67 mg g^-1, with the highest content being recorded in a 70% EtOH extract of Desmarestia tabacoides (81.67 mg g^-1), followed by that of Agarum clathratum (78.70 mg g^-1). Conclusions: The results indicate that 70% EtOH extracts of D. tabacoides and A. clathratum containing fucosterol with various effects can be potential alternative sources of fucosterol.

• Korean Journal of Environmental Agriculture
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• v.33 no.4
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• pp.414-418
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• 2014

BACKGROUND: Benzene, toluene, ethylbenzene and xylene (BTEX), which are volatile aromatic hydrocarbons and main constituents of gasoline, are neuro-carcinogenic organic pollutants in soil and groundwater. Korea Ministry of Environment has established the maximum permissible level of BTEX in arable soil to 1, 20, 50 and 15 mg/kg, respectively. METHODS AND RESULTS: To understand an arable soil contamination by BTEX, we collected 92 samples from the arable lands around oil reservoir, and analyzed the BTEX residue using a GC-MS with head-space sampler. A linear correlation between BTEX concentration and peak areas was detected with coefficient correlations in the range of 0.9807-0.9995. The method LOQ of BTEX was 0.002, 0.014, 0.084, and 0.038 mg/kg, respectively. Recoveries of 0.5 mg/kg BTEX were found to be 73.7-96.9%. The precision was reliable since RSD percentage (0.7-7.5%) was below 30, which was the normal percent value. Also, BTEX in all samples were detected under the LOQ. CONCLUSION: These results showed that the investigated arable soils around airport and oil reservoir in Korea were not contaminated by oils.

• Mass Spectrometry Letters
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• v.8 no.1
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• pp.18-22
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• 2017

Products containing any one or more of 26 fragrance allergens likely to cause contact allergies, are required under the 2008 domestic cosmetic law to be labeled when their concentrations exceed a certain range. This study focuses on the comparison and development of analytical methods based on headspace-solid phase micro extraction (HS-SPME) and liquid-liquid extraction (LLE) methods followed by GC-MS/MS for 24 of the fragrance allergens excepting for two natural materials in water samples. Using the developed HS-SPME method, 15 of the 24 fragrance allergens were analyzed and 9 compounds which have relatively low $logK_{OW}$ values (below about 2.5) were not extracted, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9969 or more, and the method detection limits (MDL) and the limits of quantification (LOQ) were $0.078{\sim}0.582{\mu}g/L$ and $0.261{\sim}1.940{\mu}g/L$, respectively. In the case of using the optimized LLE method, all 24 fragrance allergens were analyzed, and the correlation coefficient ($r^2$) of the calibration curve for quantification showed linearity of 0.9957 or more, MDL and LOQ were $0.020{\sim}0.138{\mu}g/L$ and $0.065{\sim}0.440{\mu}g/L$, respectively.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.46 no.2
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• pp.147-153
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• 2013

To prevent paralytic shellfish poisoning (PSP) due to the consumption of shellfish contaminated with PSP toxins, the quantitative analysis of these toxins is very crucial. The AOAC International mouse bioassay (MBA) has been used widely for the routine monitoring of PSP toxins for more than 50 years. However, this method has low sensitivity and high limit of quantification (LOQ) and interferences from other components in the extract, and it cannot determine toxic profiles. Ethical problems also exist with the continued use of this live mouse assay. To establish an alternative method to the MBA used for PSP toxins analysis, we attempted to optimize the analysis conditions of a precolumn high-performance liquid chromatography (HPLC) oxidation method and succeeded in validating its accuracy and precision in quantifying PSP toxins. A clear peak and the isolation of PSP toxins were obtained by injecting the working standards of Certified Reference Materials using HPLC. The LOQ of the precolumn HPLC oxidation method for PSP toxins was about $0.1002{\mu}g/g$, which represented an approximately fourfold improvement in detection capability versus the AOAC MBA. The intra-accuracy and precision for PSP toxins in oysters were 77.0-103.3% and 2.0-5.7%, respectively, while the respective inter-accuracy and precision were 77.3-100.7% and 2.4-6.0%. The mean recoveries of PSP toxins from oysters were 75.2-112.1%. The results of a comparison study showed good correlation between the results of the precolumn HPLC oxidation method and those of MBA, with a correlation factor of 0.9291 for mussels. The precolumn HPLC oxidation method may be used as an alternative to, or supplementary method with, MBA to monitor the occurrence of PSP toxins and to analyze the profiles of these toxins in shellfish.

• Journal of Genetic Medicine
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• v.12 no.2
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• pp.79-84
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• 2015

Purpose: We developed and validated a fetal trisomy detection method for use as a noninvasive prenatal test (NIPT) including a Clinical Laboratory Improvement Amendments (CLIA)-certified bioinformatics pipeline on a cloud-based computing system using both Illumina and Life Technology sequencing platforms for 221 Korean clinical samples. We determined the necessary proportions of the fetal fraction in the cell-free DNA (cfDNA) sample for NIPT of trisomies 13, 18, and 21 through a limit of quantification (LOQ) test. Materials and Methods: Next-generation sequencing libraries from 221 clinical samples and three positive controls were generated using Illumina and Life Technology chemistries. Sequencing results were uploaded to a cloud and mapped on the human reference genome (GRCh37/hg19) using bioinformatics tools. Based on Z-scores calculated by normalization of the mapped read counts, final aneuploidy reports were automatically generated for fetal aneuploidy determination. Results: We identified in total 29 aneuploid samples, and additional analytical methods performed to confirm the results showed that one of these was a false-positive. The LOQ test showed that the proportion of fetal fraction in the cfDNA sample would affect the interpretation of the aneuploidy results. Conclusion: Noninvasive chromosome examination (NICE), a CLIA-certified NIPT with a cloud-based bioinformatics platform, showed unambiguous success in fetus aneuploidy detection.

• YAKHAK HOEJI
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• v.54 no.6
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• pp.429-440
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• 2010

HS-SPME-GC/MS was studied and optimized for the determination of 17 orgarnophosphorous pesiticides (OPPs: chlorpyrifos, chlorpyrifos-methyl, demeton-s-methyl, diazinon, dimethoate, EPN, fenitrothion, fenthion, malathion, methidathion, monocrotophos, parathion, phenthoate, phosphamidon, sulfotep, terbufos, triazophos) in blood. Optimum SPME parameters were selected: choice of SPME fiber (85 ${\mu}m$ polyacrylate), pH effect (0.5 N HCl), salt effect ($Na_2SO_4$, 0.2 g; 20%), headspace incubation temperature ($80^{\circ}C$), headspace incubation time (1 min), headspace adsorption time (30 min) and GC desorption time (2 min). These parameters were optimized using HS-SPME autosampler coupled with gas chromatography-mass spectrometry (GC-MS). Method validation was carried out in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ) and recovery in blood. The assay was linear over 0.5~5.0 mg/l ($r^2$=0.955~1.000). Limit of detection (LOD) and limit of quantitation (LOQ) in blood were determined 0.03~0.3 mg/l (S/N=3) and 0.1~1.1 mg/l (S/N=10), respectively. Relative recovery with 0.5, 1 and 5 mg/l (in blood) were 90.8%, 98.5% and 94.1%, respectively. This method will be applied to the determination of the orgarnophosphorous pesticides in postmortem blood. The proposed protocol can be an attractive alternative to be used in routine toxicological analysis.

• Korean journal of food and cookery science
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• v.31 no.2
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• pp.112-117
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• 2015

The analytical method for ethyl carbamate (EC) in maesil (Prunus mume) extract was developed with deuterium-labeled ethyl carbamate as an internal standard. Samples were neutralized with an addition of 1 N sodium hydroxide solution, followed by a solid phase extraction with a Chem Elut cartridge. A standard curve exhibited a good linearity with correlation coefficient of 0.9991. The limit of detection (LOD) and limit of quantification (LOQ) were 2.91 ng/g and 8.83 ng/g, respectively. The recovery rate of EC ranged from 91.40% to 120.90%. The precision never exceeded 12.57% (intra-day) and 11.03% (inter-day). Samples were comprised of 24 home-made and 7 commercially-available maesil extracts. Eight home-made samples contained EC at levels between 3.39 and 75.76 ng/g. Three commercially-available samples had EC at levels between 11.67 and 20.16 ng/g. Average daily intakes of EC from maesil extracts for consumers were 0.23 g/kg of body weight. Based on a benchmark dose confidence limit ($BMDL_{10}$) of 0.25 mg/kg of body weight/day, the margin of exposure (MOE) of EC in maesil extract for consumers was 94,150, which is not of concern. Considering that a daily intake of maesil extract has been increasing, further studies on the formation of EC in maesil extract is needed.

• The Korea Journal of Herbology
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• v.30 no.3
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• pp.19-24
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• 2015

Objectives : HPL-1, a novel herbal medicine which is composed of five herbs such as Kalopanacis Cortex, Chaenomelis Fructus, Raphani Semen, Atractylodis Rhizoma and Pulvis Aconiti Tuberis Purificatum, was developed for treatment of osteoarthritis. This study is aimed to develop analytical method for consistent quality control of HPL-1 and validate chromatographic method. Methods : Chromatographic analysis was performed using ultra-high performance liquid chromatography - diode array detector (UHPLC-DAD) equipped with RP-amide column, column oven, and auto sampler. Marker compounds [protocatechuic acid, chlorogenic acid, liriodendrin, 3,5-dicaffeoylquinic acid, ${\beta}$-D-(3-O-sinapoyl)-fructofuranosyl-$\alpha$-D-(6-O-sinapoyl)glucopyranoside and benzoylmesaconine] were separated by step gradient elution of acetonitrile and 0.1% phosphoric acid/water. The method validation was evaluated by quantitative validation parameters of linearity, accuracy, precision, limit of detection (LOD) and limit of quantification (LOQ) according to KFDA guideline.Results : An optimized method for six marker compounds in HPL-1 was established by UHPLC-DAD. The correlation coefficient (R²) with each calibration curve was greater than 0.99. The LOD and LOQ were within the range of 0.008-0.090 and $0.023-0.274{\mu}g/mL$, respectively. The relative standard deviation (RSD) of intra- and inter-day variability were less than 4.0%. The result of recovery test was range from 93.3-106.3% with RSD < 4.0%.Conclusions : These results suggest that the quantitative UHPLC method is precise, accurate, effective for quality evaluation of HPL-1. The method may also contribute to improve quality of crude drug preparations used for treatment of various diseases.

• Korean Journal of Fisheries and Aquatic Sciences
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• v.43 no.6
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• pp.623-628
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• 2010

The distribution of fluoroquinolones was investigated in the carp (Cyprinus carpio) and eel (Anguilla japonica) after an oral dose of 20 mg/kg body weight/day for 35 days. Blood samples were collected at 5 and 10 hours and 1, 2, 3, 5, 7, 9, 13, 20, 30, and 35 days after treatment. The fluoroquinolone concentrations were determined high- performance liquid chromatography with an ultraviolet detector. The recovery rates of fluoroquinolones in the fish samples ranged from 91.4-96.6, 91.2-96.5, and 90.4-98.6% for concentrations of 0.1, 0.5, and $1.0\;{\mu}g/g$, respectively. In the blood of carp, ciprofloxacin, enrofloxacin, norfloxacin, and sarafloxacin reached maximums level of 11.03, 9.37, 9.10, and $9.81\;{\mu}g/g$ 10 hours, 1 day, 10 hours, and 10 hours after treatment, respectively. In the eel blood, these reached maximum levels of 12.65, 11.18, 11.91, and $8.74\;{\mu}g/g$ all at 10 hours. Carp sample concentrations of ciprofloxacin, enrofloxacin, norfloxacin, and sarafloxacin were not measurable 20, 30, 20, and 20 days after treatment, respectively, in all experiments (