• Journal of the Korea Institute of Military Science and Technology
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• v.13 no.3
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• pp.478-485
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• 2010

The vaccine is biological pretreatment that improves immunity to a particular disease. We can get immunity from producing antibody with injection antigen which has ability to defense against the disease. The ELISA is the most widely used method to measure antibody titer. We have developed and performed validation of ELISA according to the guideline of KFDA and ICH. In this paper, we have verified ELISA method is an excellent method to measure the titer of anti-PA antibody. We have constructed recombinant protective antigen among anthrax toxins and used as antigen of ELISA. In this validation, we have evaluated precision (repeatability, interlaboratory precision), specificity, linearity(range) and LOD, which are validation articles suggested by guideline. Inter-person precision was replaced with inter-laboratory precision. From the results, we have confirmed high precision in all experiments with CV under 20%.

• Journal of Food Hygiene and Safety
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• v.29 no.4
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• pp.285-291
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• 2014

Saflufenacil is a low-volatile and uracil-based herbicide. This herbicide is used for pre-and post-emergence control of major broadleaf weeds. The objective of present study was to develop and validate an analytical method for saflufenacil determination in agricultural products for ensuring the food safety. The saflufenacil residues in samples were extracted with acetone, dichloromethane, and then purified with silica and graphitized carbon cartridge. The purified samples were analyzed by HPLC-UVD and confirmed with LC-MS. The linear range of saflufenacil was $0.1{\sim}5.0{\mu}gmL^{-1}$ with the correlation coefficient (r) = 0.999. Average recoveries of saflufenacil ranged from 80.5% to 110.2% at the spiked level of $0.02{\sim}0.5mgkg^{-1}$, while the relative standard deviation was 0.3~7.3%. In addition, the limit of detection and limit of quantification were 0.005 and $0.02mgL^{-1}$, respectively. Furthermore, an interlaboratory study among three labs was conducted to validate the method, and the results were satisfactory.

• Journal of the Society of Cosmetic Scientists of Korea
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• v.25 no.2
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• pp.129-138
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• 1999

피부 전용 제재 개발을 위해 요구되는 동물 대체 시험법 중 가장 적극적으로 연구가 행하여지곤 실제 실용화가 예상되는 것은 안점막 자극 시험으로 지금까지 여러 가지 방법이 개발되었지만 그 중 계란 유정란의 응모요막(CAM)을 이용한 방법이 현재 가장 활발히 진행되고 있다. 이 방법이 일부 국가에서 이미 안점막 자극 시험 동물 대체 시험법으로 공인되었으며 현재까지도 validation 연구를 활발히 진행하고 있다. 본 연구에서도 국내에 적합한 안점막 자극 시험 동물 대체 시험법의 공인 시험법 개발 및 validation study를 목표로 계란 유정란의 응모요막을 이용한 방법 중 HET-CAM 방법을 시행하였으며 안점막 동물 대체 시험법으로 확립하고자 하였다. 틴ET-CAM 방법의 보완을 위해 배양된 세포를 통해 자극도를 측정할 수 있는 방법인 Cytotoxicity test를 도입하여 시행하였으며 두 방법의 data들을 분석하여 validation study를 수행하였다. 국내 유수의 6개 장업사가 본 연구에 참가하여 20가지의 화장품 전용제재를 대상으로 1차, 2차 validation study 를 진행하였다. HET-CAM test, Draize eye irritation test, Cytotoxicity test 측정 결과 HET-CAM 의 “Q” 수치는 대부분 강자극 수치인 2 이상이었고 10% sodium hydroxide가 가장 높은 수치를 보였으며 Tween 20(sorbitanpolyoxyethylene monolaurate) 100%가 가장 낮은 수치를 보였다. In vi패의 경우 10% sodium hydroxide가 가장 높은 수치를 보였으며 30군 propylene glycol 이 가장 낮은 자극수치를 보였다. HET-CAM test 와 Draize eye irritation test, Cytotoxicity test 간의 상관성 분석은 linear correlation coefficient 와 rank correlation coefficient를 구하여 비교하였으며 6개 장업사(A-F)의 실험실에서의 HET-CAM test 결과를 취합하여 각각 두 실험실간의 상관관계(linear correlation)를 분석하였다. Linear correlation coefficient 분석 결과를 보면 전반적으로 상관관계가 0.589 - 0.954의 범위였으며, 특히 A사와 B사 사이의 경우 0.954이었으며, E사와 D사 사이의 경우 0.942로 높은 상관관계를 보였다. 그 외에도 A사와 D사 사이의 경우(0.589)와 B사와 D사 사이의 경우(0.638)를 제외하고는 대체로 높은 상관관계를 나타내었다.

• Journal of Korean Society for Atmospheric Environment
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• v.16 no.5
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• pp.453-467
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• 2000

The aim of this research is to collect and characterize fine particles (FPM:$\leq$2.5${\mu}{\textrm}{m}$) and coarse particles (CPM: 2.5~10${\mu}{\textrm}{m}$) using a low volume air sampler provided by the IAEA, at urban (Taejon) and rural area(Wonju) for a period of about two years(April 1996 to May 1998) and to promote a use of nuclear analytical techniques for air pollution studies. For the collection of airborne particulate matter (PM(sub)10), the Gent stacked filter unit sampler and polycarbonate membrane filters were employed. The concentration of trace elements in collected APM samples were determined byu instrumental Neutron Activation Analysis. For validation of the analytical data, internal quality control were implemented by using both the comparison of the analytical results of standard reference materials(NIST SRM 1648) and interlaboratory comparison for proficiency test (NAT-3). The standard uncertainty was less than 15% and Z-score of two samples were within $\pm$1. The monitoring of (PM(sub)10) mass concentration and elemental concentrations were carried out weekly. The average mass concentration of (PM(sub)10) in urban and rural areas were 59.2$\pm$36.5$\mu\textrm{g}$/㎥ and 41.4$\pm$23.7$\mu\textrm{g}$/㎥, respectively. To investigate the emission source, the enrichment factors were calculated for the fine and coarse particle fractions at two sites, respectively and these values were classified for anthropogenic and soil origin elements.

• Analytical Science and Technology
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• v.36 no.3
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• pp.105-112
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• 2023

Lycopene, a carotenoid hydrocarbon is known to have effects on reducing cardiovascular risk factors, blood lipids, and blood pressure. Thus, a lot of supplementary foods with lycopene in several dosage forms like soft capsule filled with liquid and hard capsule filled with powder are available in a market. Recently, however, our research group found that the lycopene assay in Supplementary Food Code of South Korea is only valid for oily lycopene preparation. Thus, here, we developed a simple method to determine lycopene in solid preparations for Supplementary Food Code of South Korea using saponification and liquid chromatography with an absorbance detector. The method was validated following Ministry of Food and Drug Safety guidelines. All validation parameters observed in this study were within acceptable criteria of the guidelines (selectivity, linearity of r² ≥ 0.991, lower limit of quantification of 0.0149 mg/mL, accuracy as recovery (R) between 92.70 and 97.18 %, repeatability as relative standard deviation (RSD) values of R between 0.85 and 1.59 %, and reproducibility as the RSD value of interlaboratory R of 3.70 %). Additionally, the practical sample applicability of the validated method was confirmed by accuracy between 98.81 and 101.59 % observed from its lycopene certified reference material (CRM) analyses. Therefore, the present method could contribute to fortify the supplementary food safety management system in South Korea.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.298-305
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• 2017

Benzovindiflupyr is a new pyrazole carboxamide fungicide that inhibits succinate dehydrogenase of mitochondrial respiratory chain. This study was carried out to develop an analytical method for the determination of benzovindiflupyr residues in agricultural commodities using LC-MS/MS. The benzovindiflupyr residues in samples were extracted by using acetonitrile, partitioned with dichloromethane, and then purified with silica solid phase extraction (SPE) cartridge. Correlation coefficient ($r^2$) of benzovindiflupyr standard solution was 0.99 over the calibration ranges ($0.001{\sim}0.5{\mu}g/mL$). Recovery tests were conducted on 5 representative agricultural commodities (mandarin, green pepper, potato, soybean, and hulled rice) to validate the analytical method. The recoveries ranged from 79.3% to 110.0% and then relative standard deviation (RSD) was less than 9.1%. Also the limit of detection (LOD) and limit of quantification (LOQ) were 0.0005 and 0.005 mg/kg, respectively. The recoveries of interlaboratory validation ranged from 83.4% to 117.3% and the coefficient of variation (CV) was 9.0%. All results were followed with Codex guideline (CAC/GL 40) and Ministry of Food and Safety guideline (MFDS, 2016). The proposed new analytical method proved to be accurate, effective, and sensitive for benzovindiflupyr determination and would be used as an official analytical method.

• Journal of Food Hygiene and Safety
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• v.37 no.6
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• pp.373-384
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• 2022

Fluoxastrobin a fungicide developed from Strobilurus species mushroom extracts, can be used as an effective pesticide to control fungal diseases. In this study, we optimized the extraction and purification of fluoxastrobin according to its physical and chemical properties using the QuEChERS method and developed an LC-MS/MS-based analysis method. For extraction, we used acetonitrile as the extraction solvent, along with MgSO₄ and PSA. The limit of quantitation of fluoxastrobin was 0.01 mg/kg. We used 0.01, 0.1, and 0.5 mg/kg of five representative agricultural products and treated them with fluoxastrobin. The coefficients of determination (R²) of fluoxastrobin and fluoxastrobin Z isomer were > 0.998. The average recovery rates of fluoxastrobin (n=5) and fluoxastrobin Z isomer were 75.5-100.3% and 75.0-103.9%, respectively. The relative standard deviations (RSDs) were < 5.5% and < 4.3% for fluoxastrobin and fluoxastrobin Z isomer, respectively. We also performed an interlaboratory validation at Gwangju Regional Food and Drug Administration and compared the recovery rates and RSDs obtained for fluoxastrobin and fluoxastrobin Z isomer at the external lab with our results to validate our analysis method. In the external lab, the average recovery rates and RSDs of fluoxastrobin and fluoxastrobin Z isomer at each concentration were 79.5-100.5% and 78.8-104.7% and < 18.1% and < 10.2%, respectively. In all treatment groups, the concentrations were less than those described by the 'Codex Alimentarius Commission' and the 'Standard procedure for preparing test methods for food, etc.'. Therefore, fluoxastrobin is safe for use as a pesticide.

• Journal of Food Hygiene and Safety
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• v.32 no.4
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• pp.290-297
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• 2017

The purpose of this study was developed for the determination of tridemorph in agricultural commodities samples. Tridemorph residues in samples were extracted with acetonitrile, partitioned with saline water, and then purified using and aminopropyl ($NH_2$) SPE catridge. The purified samples were quantified and confirmed via liquid chromatograph-tandem mass spectrometer (LC-MS/MS) in positive ion mode using multiple reaction monitoring (MRM). Matrix-matched calibration curves were linear over the calibration ranges (0.005~2.5 ng) into a blank extract with $r^2$ > 0.999. The limits of detection and quantification were 0.001 and 0.005 mg/kg, respectively. The average recovery ranged between 75.9% and 103.7% at different concentration levels (LOQ, 10 LOQ, 50 LOQ, n = 5) with relative standard deviations (RSDs) less than 9.0%. An interlaboratory study was conducted to validate the method by Korea Advanced Food Research Institute. The average recovery ranged between 87.0% and 109.2% at different concentration levels (LOQ, $10{\times}LOQ$, $50{\times}LOQ$, n = 5) with relative standard deviations (RSDs) less than 8.0%. All values were consistent with the criteria ranges requested in the Codex guidelines (CAC/GL40, 2003) and Food Safety Evaluation Department guidelines (2016). The results prove that the developed analytical methods is accurate, effective and sensitive for tridemorph determination.