• 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.

• Analytical Science and Technology
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• v.27 no.2
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• pp.92-99
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• 2014

Interferences were removed using anion exchange solid phase extraction (AE SPE) in quantification of selenoproteins in Korean human blood serum with affinity high performance liquid chromatography (AF HPLC)-inductively coupled plasma/mass spectrometry (ICP/MS). The average selenium level obtained for healthy Koreans was $94.3{\pm}2.3ngg^{-1}$ using isotope dilution method. AE SPE was coupled to AF column to separate 3 selenoproteins, glutathione peroxidase GPx, selenoprotein SelP, and selenoalbumin SeAlb. Post column isotope dilution was employed to quantify the proteins. The certified reference material of human blood serum BCR-637 was analyzed to give total selenoprotein concentration of $85.4{\pm}3.4ngg^{-1}$, which agreed well with the reference value of $81{\pm}7ngg^{-1}$. The pooled concentration of GPx, SelP, and SeAlb from healthy Koreans (n=20) was $12.1{\pm}1.4ngg^{-1}$, $57.2{\pm}2.0ngg^{-1}$, and $20.0{\pm}1.9ngg^{-1}$, respectively. The sum of selenoproteins is $89.3ngg^{-1}$, which is about the same as the total selenium concentration of $94.3ngg^{-1}$. The fact suggests that selenium in blood serum is mostly consisted of selenoproteins. After the removal of interference, GPx showed a significant decrease (more than 50%) from $25.0ngg^{-1}$ to $12.1ngg^{-1}$. It was identified that the interference in blood serum was mostly from GPx and the use of AE SPE was proven to be efficient in eliminating Cl and Br that cause interference to GPx.

• Journal of Food Hygiene and Safety
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• v.34 no.5
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• pp.454-462
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• 2019

A conventional Korean meal typically includes various roasted, steamed, stir-fried, and braised foods. For this study, we investigated the contents of water soluble vitamins, $B_1$ (thiamin), $B_2$ (riboflavin) and $B_3$ (niacin) in various roasted, steamed, stir-fried, and braised foods. Method validation for analytical data in this study showed a high linearity ($r^2$>0.999), and the limit of detection and quantification were 0.001-0.067 and $0.002-0.203{\mu}g/mL$, respectively. For accuracy and precision, analytical values using standard reference materials were in the certified ranges. Roasted foods contained 0.039-1.057 mg/100 g of thiamin, 0.058-0.686 mg/100 g of riboflavin and 0.021-21.772 mg/100 g of niacin. Steamed foods contained 0.049-1.066 mg/100 g of thiamin, 0.025-0.548 mg/100 g of riboflavin and 0.134-21.509 mg/100 g of niacin. Stir-fried foods contained 0.114-0.388 mg/100 g of thiamin, 0.014-1.258 mg/100 g of riboflavin and 0.015-2.319 mg/100 g of niacin. Braised foods contained 0.112-1.656 mg/100 g of thiamin, 0.024-0.298 mg/100 g of riboflavin and 0.322-2.157 mg/100 g of niacin. The data on water-soluble vitamins in this study can be used for a nutritional database of conventional Korean meals.

• 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.

• 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 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.