• Title/Summary/Keyword: 4/2 SRM

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Improvement of Analysis Methods for Fatty Acids in Infant Formula by Gas Chromatography Flame-Ionization Detector (GC-FID를 이용한 조제유류 중 지방산 분석법 개선 연구)

  • Hwang, Keum Hee;Choi, Won Hee;Hu, Soo Jung;Lee, Hye young;Hwang, Kyung Mi
    • Journal of Food Hygiene and Safety
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    • v.36 no.1
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    • pp.34-41
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    • 2021
  • The purpose of this research is to improve analysis methods of determining the contents of fatty acids in infant formulas and follow-up formulas. A gas chromatography (GC) method was performed on a GC system coupled to flame ionization detector, with a fused silica capillary column (SP2560, 100 m×0.25 mm, 0.20 ㎛). The method was validated using standard reference material (SRM, NIST 1849a). Performance parameters for method validation such as specificity, linearity, limits of detection (LOD) and quantification (LOQ), accuracy and precision were examined. The linearity of standard solution with correlation coefficient was higher than 0.999 in the range of 0.1-5 mg/mL. The LOD and LOQ were 0.01-0.06 mg/mL and 0.03-0.2 mg/mL, respectively. The recovery using standard reference material was confirmed and the precision was found to be between 0.8% and 2.9% relative standard deviation (RSD). Optimized methods were applied in sample analysis to verify the reliability. All the tested products had acceptable contents of fatty acids compared with component specification for nutrition labeling. The result of this research will provide efficient experimental information and strengthen the management of nutrients in infant formula and follow-up formula.

Development of Vitamin D Determination in Infant Formula by Column-Switching HPLC with UV Detector

  • Ko, Jin-Hyouk;Kwak, Byung-Man;Ahn, Jang-Hyuk;Shim, Sung-Lye;Kim, Kyong-Su;Yoon, Tae-Hyung;Leem, Dong-Gil;Jeong, Ja-Young
    • 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.

Vitamin D analysis in the Korean total diet study and UV/sun light irradiated mushrooms (한국형 총식이조사 및 UV/태양광 조사 버섯에서의 비타민 D 분석)

  • Min-Jeong Seo;In-Hwa Roh;Jee-Yeon Lee;Sung-Ok Kwon;Cho-Il Kim;Gae-Ho Lee
    • 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.

Vitamin B5 and B6 Contents in Fresh Materials and after Parboiling Treatment in Harvested Vegetables (채소류의 수확 후 원재료 및 데침 처리에 의한 비타민 B5 및 B6 함량 변화)

  • Kim, Gi-Ppeum;Ahn, Kyung-Geun;Kim, Gyeong-Ha;Hwang, Young-Sun;Kang, In-Kyu;Choi, Youngmin;Kim, Haeng-Ran;Choung, Myoung-Gun
    • Horticultural Science & Technology
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    • v.34 no.1
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    • pp.172-182
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    • 2016
  • This study was aimed to determine the changes in vitamin $B_5$ and $B_6$ contents compared to fresh materials after parboiling treatment of the main vegetables consumed in Korea. The specificity of accuracy and precision for vitamin $B_5$ and $B_6$ analysis method were validated using high-performance liquid chromatography (HPLC). The recovery rate of standard reference material (SRM) was excellent, and all analysis was under the control line based on the quality control chart for vitamin $B_5$ and $B_6$. The Z-score for vitamin $B_6$ in food analysis performance assessment scheme (FAPAS) proficiency test was -1.0, confirming reliability of analytical performance. The vitamin $B_5$ and $B_6$ contents in a total of 39 fresh materials and parboiled samples were analyzed. The contents of vitamin $B_5$ and $B_6$ ranged from 0.000 to 2.462 and from 0.000 to $0.127mg{\cdot}100g^{-1}$, respectively. The highest contents of vitamin $B_5$ and $B_6$ were $2.462mg{\cdot}100g^{-1}$ in fresh fatsia shoots (stem vegetables), and $0.127mg{\cdot}100g^{-1}$ in fresh spinach beet (leafy vegetables), respectively. Moreover, the vitamin $B_5$ and $B_6$ contents for parboiling treatment in most vegetables were reduced or not detected. In particular, the contents of vitamin $B_5$ in parboiled fatsia shoots and vitamin $B_6$ in parboiled yellow potato and spinach beet were decreased 20- and 4-fold compared with fresh material, respectively. These results can be used as important basic data for utilization and processing of various vegetable crops, information for dietary life, management of school meals, and national health for Koreans.

Quantifying Uncertainty of Vitamin C Determination in Infant Formula by Indophenol Titration Method (인도페놀 적정법에 의한 성장기용조제식 중 비타민 C 함량분석의 측정불확도 산정)

  • Jun, Jang-Young;Kwak, Byung-Man;Ahn, Jang-Hyuk;Kong, Un-Young
    • 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.