• Food Science of Animal Resources
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• v.32 no.5
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• pp.571-577
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• 2012

This study was carried out to develop an analytical method for the determination of vitamin D in infant formula. Vitamin D was determined by column-switching high-performance liquid chromatography (HPLC) equipped with a reversed phase column and UV detector after saponification and extraction of the formula with an organic solvent. A preseparation column ($C_8$), focusing column ($C_{18}$), analytical column ($C_{18}$) and UV-Vis detector (254 nm) were used. The limits of detection (LOD) and the limits of quantification (LOQ) for vitamin D were estimated to be $1.51{\mu}g/kg$ and $4.95{\mu}g/kg$, respectively. The linearity, recovery, precision and accuracy of the analytical method for vitamin D were evaluated through the application of a SRM (Standard Reference Material) 1846 (National Institute of Standard & Technology, USA). The linearity of this method was calculated with a value of the coefficient of determination ($r^2$) ${\geq}0.9999$. The recovery of vitamin D was $85.20{\pm}3.00%$. The intra-assay precision for vitamin D was between $1.68{\pm}0.03%$ and $5.75{\pm}0.33%$, and the inter-assay precision for vitamin D ranged from $1.73{\pm}0.03%$ to $2.96{\pm}0.09%$. The intra-assay accuracy for vitamin D was between $100.03{\pm}2.77%$ and $102.01{\pm}0.59%$, and the inter-assay accuracy for vitamin D ranged from $99.00{\pm}1.53%$ to $102.01{\pm}3.04%$. The proposed method is optimal for the separation and quantification of vitamin D from infant formula.

• Food Science and Preservation
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• v.30 no.1
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• pp.109-121
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• 2023

This study was conducted to evaluate vitamin D intake of Koreans in a total diet study (TDS) and to determine the effect of irradiation on vitamin D synthesis in mushrooms. For analysis, sample were saponified and extracted with hexane, and vitamin D was quantified by liquid chromatography-tandem mass spectrometry (LC-MS/MS). Based on the validation results, the recovery of the National Institute of Standards and Technology (NIST) standard reference sample (SRM) 1849a was 96.7% and the z-score of -1.6 was obtained by the Food Analysis Performance Assessment Scheme (FAPAS) proficiency test (PT) 21115. Vitamin D₂ was not detected in any samples, and the highest level of vitamin D₃ was detected in mackerel and anchovies ranging from 24.2 to 120.2 ㎍/kg. The mean daily intake of vitamin D was 0.99 ㎍/day, as estimated from the vitamin D contents of the analyzed foods and their corresponding intake. The adequate intake (AI) of vitamin D based on the Dietary reference intakes for Koreans provided by the Ministry of Health and Welfare is 5-15 ㎍/day for Koreans aged 6 to 75 years. Compared with this AI, vitamin D intake of Koreans estimated in this study was inadequate. For that, the increased vitamin D content in ultraviolet (UV)/sun light irradiated mushrooms warrants further research to increase vitamin D intake of Koreans through diet.

• Korean Journal of Food Science and Technology
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• v.37 no.3
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• pp.352-359
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• 2005

Uncertainty involved during determination of vitamin C content in infant formula was quantified by indophenol titration method. Uncertainty sources in measurand, such as purity, weight, final volume of standard, volume of standard solution used for titration, sample weight, final volume of sample, extraction solution used for titration, titration of extraction solution and standard solution by indophenol solution were identified and used as parameters for combined standard uncertainty based on Guide to the expression of uncertainty in measurement (GUM) and Draft EURACHEM/CITAC Guide. Uncertainty parameters of each source in measurand were identified as resolution, reproducibility and stability of chemical balance, standard material purity, repeatability, reproducibility, end point of titration, 1 mL pipet, 5 mL autopipet, and 100 mL mass flask. Each uncertainty component was evaluated by types A and B and included to calculate combined uncertainty. Analytical test result for traceability under laboratorial conditions using Certified Reference Material (CRM) test was certified as $108.4{\pm}1.7mg/100g$, which was within CRM certification range of $114.6{\pm}6.6mg/100g$. Uncertainty test result of vitamin C content of 5 g sampling was $56.7{\pm}2.44mg/100g$. Uncertainty could be reduced by identification of uncertainty sources and components related with vitamin C determination by indophenol titration method and by decreasing uncertainty sources and components.