• Journal of Food Hygiene and Safety
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• v.32 no.5
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• pp.411-417
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• 2017

This study was conducted to establish the analysis method for the contents of choline in infant formulas and follow-up formulas by ion chromatograph (IC). To optimize the method, we compared several conditions for extraction, purification and instrumental measurement using spiked samples and certified reference material (CRM; NIST SRM 1849a) as test materials. IC method for choline was established using Ion Pac CG column and 18 mM $H_2SO_4$ mobile phase. The parameters of validation were specificity, linearity, LOD, LOQ, recovery, accuracy, precision and repeatability. The specificity was confirmed by the retention time and the linearity, $R_2$ was over 0.999 in range of 0.5~10 mg/L. The detection limit and quantification limit were 0.14, 0.43 mg/L. The accuracy and precision of this method using CRM were 95%, 2.1% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested products were acceptable contents of choline compared with component specification for nutrition labeling. The standard operating procedures were prepared for choline to provide experimental information and to strengthen the management of nutrient in infant formula and follow-up formula.

• Korean Journal of Food Science and Technology
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• v.36 no.5
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• pp.701-710
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• 2004

Uncertainty was quantified to evaluate calcium determination result in infant formula with AAS (Atomic Absorption Spectrometry) and ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry). Uncertainty sources in measurand, such as sample weight, final volume of sample, sample dilution and the instrumental result were identified and used as parameters for combined standard uncertainty based on the GUM (Guide to the expression of uncertainty in measurement) and Draft EURACHEM/CITAC Guide. Uncertainty components of each sources in measurand were identified as resolution, reproducibility and stability of chemical balance, standard material purity, standard material molecular weight, standard solution concentration, standard solution dilution factor, sample dilution factor, calibration curve, recovery, instrumental precision, reproducibility, and stability, Each uncertainty components were evaluated by uncertainty types and included to calculate combined uncertainty. The kinds of uncertainty sources and components in the analytical method by AAS and ICP-AES were same except sample dilution factor for AAS. The analytical results and combined standard uncertainties of calcium content were estimated within the certification range $(367{\pm}20\;mg/100g)$ of CRM (Certified Reference Material) and were not significantly different between method by AAS followed by ashing and method by ICP-AES followed by acid digestion as $359.52{\pm}23.61\;mg/100g\;and\;354.75{\pm}16.16\;mg/100g$, respectively. Identifying uncertainty sources related with precision, repeatability, stability, and maintaining proper instrumental conditions as well as personal proficiency was needed to reduce analytical error.

• Journal of Food Hygiene and Safety
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• v.31 no.5
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• pp.327-334
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• 2016

This study was conducted to establish the standard method for the contents of biotin in milk formulas. To optimize the method, we compared several conditions for liquid extraction, purification and instrumental measurement using spiked samples and certified reference material (NIST SRM 1849a) as test materials. LC-MS/MS method for biotin was established using $C_{18}$ column and binary gradient 0.1% formic acid/acetonitrile, 0.1% formic acid/water mobile phase is applied for biotin. Product-ion traces at m/z 245.1 ${\rightarrow}$ 227.1, 166.1 are used for quantitative analysis of biotin. The linearity was over $R^2=0.999$ in range of $5{\sim}60{\mu}g/L$. For purification, chloroform was used as a solvent for eliminating lipids in milk formula. The linearity was over 0.999 in range of 5~60 ng/mL. The detection limit and quantification limit were 0.10, 0.31 ng/mL. The accuracy and precision of LC-MS/MS method using CRM were 103%, 2.5% respectively. Optimized methods were applied in sample analysis to verify the reliability. All the tested milk formulas were acceptable contents of biotin compared with component specification and standards for nutrition labeling. The standard operating procedures were prepared for biotin to provide experimental information and to strengthen the management of nutrient in milk formula.

• Bulletin of the Korean Chemical Society
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• v.35 no.11
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• pp.3289-3293
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• 2014

Femtosecond laser ablation (fs LA) was used in this study to identify pollution by heavy metals and the distribution of elemental nutrients at different rice milling ratios. Polished rice (degrees of milling of 3, 5, 7, 9, and 11) was collected from major Korean supermarkets and one sample thereof was selected. An internal quality control experiment was conducted using a rice flour certified reference material from the Korea Research Institute of Standards and Science (KRISS CRM) for the evaluation of the efficacy. To assess the effectiveness of the analysis method, the reliability was validated using a food analysis performance assessment scheme (FAPAS), with chili powder serving as an external quality control. The results of the analysis of the inorganic elements Ti, Ca, Al, Fe and Mn in white and brown rice with degrees of milling of 3, 5, 7, 9 and 11 using ICP-MS, ICP-OES and AAS revealed contents of 0.40, 49.2, 2.43, 5.36 and 10.3 mg/kg in white rice and 0.59, 78.0, 7.52, 11.0 and 18.5 mg/kg in brown rice, respectively. Among the elements, there were remarkable differences in the measured contents. By comparing the contents of the elements at different degrees of milling, Ti, Co, As, Ca, Al, Cu, Fe, and Mn were determined to be distributed on the surface of the rice grains, whereas the contents of Cd and Pb increased toward the center of the rice grains, and Si was evenly distributed. After the quantitative analysis of rice samples polished to different degrees of milling, Ca and Al, which were contained in large amounts, and Si were analyzed with specificity by fs LA. The results show that Ca and Al were distributed in the rice husk (protective covering of rice) and Si was distributed in all parts of the rice.

• Progress in Medical Physics
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• v.25 no.1
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• pp.8-14
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• 2014

The amounts of radioactive wastes to be disposed in the medical institute have been increased due to development of radiation diagnosis and therapy rapidly. They are produced mostly by the very short lived radioisotopes such as $^{18}F$ used in PET/CT, $^{99m}Tc$, $^{123}I$, $^{125}I$ and $^{201}Tl$, etc. IAEA proposed a criteria for the clearance level of waste which depends on the individual ($10{\mu}Sv/y$) and collective dose (1 man-Sv/y), and concentration of each nuclide (IAEA Safety Series No 111-P-1.1, 1992 and IAEA RS-G-1.7, 2004). Radioactive wastes of $^{18}F$, $^{99m}Tc$, $^{123}I$, $^{125}I$ and $^{201}TI$ in the several types of container like Marinelli beaker, vial and plastic, were collected to measure the concentration of the waste of each nuclide in accordance with IAEA criteria. The measurement method and procedure of determining specific activity of the wastes using gamma emitters like MCA, gamma counter and beta emitters were developed. For the efficiency calibration of the detectors, CRM (certified reference material) which has the same dimension and shape was provided by Korea Research Institute of Standards and Science (KRISS). Correction factor of the radioactivity decay was calculated based on the measurement results, and the consideration of mutual relation with theoretical equation. The result of this study will be proposed as ISO standard.

• 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.

• Progress in Medical Physics
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• v.33 no.4
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• pp.129-135
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• 2022

Purpose: A full-energy-peak (FEP) efficiency correction is required through a Monte Carlo simulation for accurate radioactivity measurement, considering the geometrical characteristics of the detector and the sample. However, a relative deviation (RD) occurs between the measurement and calculation efficiencies when modeling using the data provided by the manufacturers due to the randomly generated dead layer. This study aims to optimize the structure of the detector by determining the dead layer thickness based on Monte Carlo simulation. Methods: The high-purity germanium (HPGe) detector used in this study was a coaxial p-type GC2518 model, and a certified reference material (CRM) was used to measure the FEP efficiency. Using the MC N-Particle Transport Code (MCNP) code, the FEP efficiency was calculated by increasing the thickness of the outer and inner dead layer in proportion to the thickness of the electrode. Results: As the thickness of the outer and inner dead layer increased by 0.1 mm and 0.1 ㎛, the efficiency difference decreased by 2.43% on average up to 1.0 mm and 1.0 ㎛ and increased by 1.86% thereafter. Therefore, the structure of the detector was optimized by determining 1.0 mm and 1.0 ㎛ as thickness of the dead layer. Conclusions: The effect of the dead layer on the FEP efficiency was evaluated, and an excellent agreement between the measured and calculated efficiencies was confirmed with RDs of less than 4%. It suggests that the optimized HPGe detector can be used to measure the accurate radioactivity using in dismantling and disposing medical linear accelerators.

• Korean Journal of Environmental Agriculture
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• v.30 no.2
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• pp.169-178
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• 2011

BACKGROUND: This study aimed to estimate the measurement uncertainty associated with determination of cadmium and lead from tomato paste by ICP/MS. The sources of measurement uncertainty (i.e. sample weight, final volume, standard weight, purity, molecular weight, working standard solution, calibration curve, recovery and repeatability) in associated with the analysis of cadmium and lead were evaluated. METHODS AND RESULTS: The guide to the expression of uncertainty was used for the GUM (Guide to the expression of Uncertainty in Measurement) and Draft EURACHEM/CITAC (EURACHEM: A network of organization for analytical chemistry in Europe/Co-Operation on International Traceability in Analytical Chemistry) Guide with mathematical calculation and statistical analysis. The uncertainty components were evaluated by either Type A or Type B methods and the combined standard uncertainty were calculated by statistical analysis using several factors. Expected uncertainty of cadmium and lead was $0.106{\pm}0.015$ mg/kg (k=2.09) and $0.302{\pm}0.029$ mg/kg (k=2.16), on basis of 95% confidence of Certified Reference Material (CRM) which was within certification range of $0.112{\pm}0.007$ mg/kg for cadmium (k=2.03) and $0.316{\pm}0.021$ mg/kg for lead (k=2.01), respectively. CONCLUSION(s): The most influential components in the uncertainty of heavy metals analysis were confirmed as recovery, standard calibration curve and standard solution were identified as the most influential components causing uncertainty of heavy metal analysis. Therefore, more careful consideration is required in these steps to reduce uncertainty of heavy metals analysis in tomato paste.

• Journal of the Korean Society of Food Science and Nutrition
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• v.39 no.6
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• pp.894-901
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• 2010

To measure the heavy metal contents of marine invertebrates, we collected 239 individuals representing 52 species from the eastern (Pohang), western (Gunsan), and southern (Tongyeong) coasts of Korea: 34 species of molluscan shellfish (Gastropoda and Bivalvia), 6 species of Cephalopoda, 8 species of Crustacea, and 4 other species. The mean levels of the heavy metals in the samples taken from the edible portion of each Gastropoda were high in the order of Zn ($21.471\;{\mu}g/g$), Cu ($4.115\;{\mu}g/g$), Mn ($0.868\;{\mu}g/g$), Ni ($0.254\;{\mu}g/g$), Pb ($0.238\;{\mu}g/g$), Cd ($0.154\;{\mu}g/g$), and Cr ($0.110\;{\mu}g/g$). The heavy metals in the Bivalvia were high in the order of Zn ($35.655\;{\mu}g/g$), Mn ($5.500\;{\mu}g/g$), Cu ($3.129\;{\mu}g/g$), Cd ($0.423\;{\mu}g/g$), Ni ($0.402\;{\mu}g/g$), Cr ($0.233\;{\mu}g/g$), and Pb ($0.232\;{\mu}g/g$). The heavy metals in the Cephalopoda were high in the order of Zn ($18.380\;{\mu}g/g$), Cu ($3.594\;{\mu}g/g$), Mn ($0.630\;{\mu}g/g$), Cr ($0.150\;{\mu}g/g$), Pb ($0.068\;{\mu}g/g$), Cd ($0.034\;{\mu}g/g$), and Ni ($0.030\;{\mu}g/g$). The heavy metals in the Crustacea were high in the order of Zn ($25.333\;{\mu}g$/g), Cu ($9.042\;{\mu}g/g$), Mn ($0.659\;{\mu}g/g$), Cr ($0.592\;{\mu}g/g$), Cd ($0.207\;{\mu}g/g$), Pb ($0.126\;{\mu}g/g$), and Ni ($0.094\;{\mu}g/g$). Therefore, the mean levels of the harmful heavy metals (Cd and Pb) in marine invertebrates were high in the order of Bivalvia>Crustacea＝Gastropoda>Cephalopoda. The average daily intakes of the heavy metals from the fisheries products were as follows: Cd ($6.88\;{\mu}g$), Cr ($19.13\;{\mu}g$), Cu ($137.02\;{\mu}g$), Mn ($156.13\;{\mu}g$), Ni ($11.39\;{\mu}g$), Pb ($7.01\;{\mu}g$) and Zn ($1,025.94\;{\mu}g$). The average weekly intakes of Cd, Cu, Pb and Zn from the fisheries products were 11.47%, 0.46%, 3.27% and 1.71% respectively, as compared with PTWI (Provisional Tolerable Weekly Intakes) established by FAO/WHO Expert Committee for Food Safety Evaluation.