• Title/Summary/Keyword: inspection.calibration

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Analytical Determination of Vitamin B12 Content in Infant and Toddler Milk Formulas by Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS)

  • Lee, Jung-Hoon;Shin, Jin-Ho;Park, Jung-Min;Kim, Ha-Jung;Ahn, Jang-Hyuk;Kwak, Byung-Man;Kim, Jin-Man
    • Food Science of Animal Resources
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    • v.35 no.6
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    • pp.765-771
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    • 2015
  • The development of a sample preparation method and optimization of the analytical instrumentation conditions were performed for the determination of the vitamin B12 content in emulsified baby foods sold on the Korea market. After removal of the milk protein and fats by chloroform extraction and centrifugation, the vitamin B12 was water extracted from the sample. Following filtration of the solution through a nylon filter, the water-soluble extract was purified by solid-phase extraction using a Liquid Chromatography Tandem Mass Spectrometry (LC-MS/MS). The solution eluted from the cartridge was dried under a stream of nitrogen gas and reconstituted with 1 mL of water. The sample solution was injected into an LC-MS/MS system after optimizing the mobile phase for vitamin B12 detection. The calibration curve showed good linearity with the coefficient of correlation (r2) value of 0.9999. The limit of detection was 0.03 µg/L and the limit of quantitation was 0.1 µg/L. The method of detection limit was 0.02 µg/kg. The vitamin B12 recovery from a spiking test was 99.62% for infant formula and 99.46% for cereal-based baby food. The sample preparation method developed in this study would be appropriate for the rapid determination of the vitamin B12 content in infant formula and baby foods with emulsified milk characteristics. The ability to obtain stable results more quickly and efficiently would also allow governments to exercise a more extensive quality control inspection and monitoring of products expected to contain vitamin B12. This method could be implemented in laboratories that require time and labor saving.

RCCA End-Tip Examination by ECT (원자로 제어봉 End-Tip 원주방향균열 와전류검사)

  • Lee, H.J.;Nam, M.W.;Jung, G.J.
    • Journal of the Korean Society for Nondestructive Testing
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    • v.18 no.6
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    • pp.455-463
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    • 1998
  • RCCA(rod cluster control assembly) End-Tip suffers from neutron irradiation and constant vibration due to high-speed internal flow of primary coolant during plant operation. Such operating conditions cause the RCCA end-tip crackings around tile circumferential weldment of the end-tip, and in some cases, the defective end-tips were completly broken loose. However, no reliable inspection techniques for end-tip crackings were developed in the past, although some techniques exist for inspecting RCCA control rod wears. Therefore, NDE group at KEPRI has developed an ECT technique for the detection and the sizing of the end-tip crackings. The technique uses a specially designed surface-riding probe that can detect size of circumferential crackings with an accuracy of ${\pm}5.31%$ RMS error. This paper describes the ECT instrumentation including the ECT probes, calibration bars, as well as technical approaches.

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A Study on the Compensation of Thermal Errors for Phase Measuring Profilometry (PMP 형상 측정법의 열 변위 보정에 관한 연구)

  • Kim, Gi-Seung;Park, Yoon-Chang
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.20 no.6
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    • pp.598-603
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    • 2019
  • Three-dimensional shape measurement technology is used in various industries. Among them, optical three-dimensional shape measurement techniques based on the optical trigonometry are mainly used in the field of semiconductor product inspection, where large quantities of three-dimensional shape measurements are made daily in factories and fine measurements are also required. The light source and the drive circuit, which are components of three-dimensional measurement equipment based on this optical trigonometry, produce heat generated by prolonged operation, and may be exposed to conditions where the ambient temperature is not constant, resulting in temperature-induced measurement errors. In this study, the compensation method of the Thermal Errors for Phase Measuring Profilometry is proposed. Three-Dimensional Shape Measurement Equipment based on Phase Measuring Profilometry is implemented to measure the height of an object and ambient temperature for 10 Hours, and a regression line was obtained line by making simple linear regression using measured temperature and height values. This regression line was used to correct the error of the height measurement according to the temperature, and thermal error was from 139.88 um(Micrometer) to 13.12 um.

Development and Validation of an Analytical Method for Determination of Fungicide Tridemorph in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 tridemorph의 시험법 개발 및 검증)

  • Pak, Won-Min;Do, Jung-Ah;Lim, Seung-Hee;Park, Shin-Min;Yoon, Ji-Hye;Lee, Dong-seouk;Chang, Moon-Ik
    • 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.

Development and Validation of Analytical Method for Nitroxoline in Chicken Using HPLC-PDA (HPLC-PDA를 이용한 닭고기 중 Nitroxoline 분석법 개발)

  • Cho, Yoon-Jae;Chae, Young-Sik;Kim, Jae-Eun;Kim, Jae-Young;Kang, Ilhyun;Lee, Sang-Mok;Do, Jung-Ah;Oh, Jae-Ho;Chang, Moon-Ik;Hong, Jin-Hwan
    • Korean Journal of Environmental Agriculture
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    • v.32 no.1
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    • pp.70-77
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    • 2013
  • BACKGROUND: Nitroxoline is an antibiotic agent. It is used for the treatment of the second bacterial infection by the colibacillosis, salmonellosis and viral disease of the poultry. When the nitroxoline is indiscreetly used, the problem about the abuse of the antibiotics can occur. Therefore, this study presented the residue analytical method of nitroxoline in food for the safety management of animal farming products. METHODS AND RESULTS: A simple, sensitive and specific method for nitroxoline in chicken muscle by high performance liquid chromatograph with PDA was developed. Sample extraction with acetonitrile, purification with SPE cartridge (MCX) were applied, then quantitation by HPLC with C18 column under the gradient condition with 0.1 % tetrabutylammonium hydroxide-phosphoric acid and methanol was performed. Standard calibration curve presented linearity with the correlation coefficient ($r^2$) > 0.999, analysed from 0.02 to 0.5 mg/L concentration. Limit of quantitation in chicken muscle showed 0.02 mg/kg, and average recoveries ranged from 72.9 to 88.1 % in chicken muscle. The repeatability of measurements expressed as coefficient of variation (CV %) was less than 12 % in 0.02 and 0.04 mg/kg. CONCLUSION(S): Newly developed method for nitroxoline in chicken muscle was applicable to food inspection with the acceptable level of sensitivity, repeatability and reproducibility.

Development and Validation of an Analytical Method for Determination of Fungicide Benzovindiflupyr in Agricultural Commodities Using LC-MS/MS (LC-MS/MS를 이용한 농산물 중 살균제 벤조빈디플루피르의 잔류시험법 개발 및 검증)

  • Lim, Seung-Hee;Do, Jung-Ah;Park, Shin-Min;Pak, Won-Min;Yoon, Ji Hye;Kim, Ji Young;Chang, Moon-Ik
    • 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.