• 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.

• Analytical Science and Technology
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• v.23 no.6
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• pp.524-530
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• 2010

Chloramphenicol is one of the most effective antibiotics for treatment of food-producing animals for typhoid fever. However, it has been reported that it caused severe side effects such as aplastic anemia in human, therefore the use of chloramphenicol for food-producing animal is prohibited by European Union and other countries. In this study, the analytical method using isotope dilution liquid chromatography-mass spectrometry (ID-LC/MS) was established for accurate determination of chloramphenicol in meat. Chloramphenicol was extracted with ethylacetate from porcine and solid phase extraction cartridge was used for enhancing the recovery. The residue of chloramphenicol in porcine was analyzed using the liquid chromatography mass spectrometer (LC/MS) interfaced with electrospray ionization source. Analysis was performed in negative mode with selected reaction mornitoring mode at m/z 321${\rightarrow}$257 of $[M-H]^-$ ${\rightarrow}$ $[M-H-(HCOCl)]^-$ and m/z 326 ${\rightarrow}$ 262 channels for its isotope. The established method was tested using fortified samples at the level of 0.2 1, 10, $25\;{\mu}g$/kg and analytical results agreed with the gravimetrically fortified values within their uncertainties. This method was validated by analyzing a certified reference material, BCR 445, from IRMM (Institute for Reference Materials and Measurement). Our measurement values agreed with the certified value within their uncertainties. The uncertainty of our measured value was much lower than that the certified value from IRMM.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.13 no.2
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• pp.113-122
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• 2015

⁵⁵Fe and ⁶³Ni are key factors in deciding the proper handling of the decommissioning of radioactive waste from nuclear facilities. For determining beta emitting radionuclides, the dismantled waste samples should be completely decomposed and separated from the sample matrix. This study reports the comparison results of the recovering efficiencies of Iron and Nickel with wet digestion methods that use various acids and alkali-fusion methods. Various matrices of NIST SRMs (1646a, 1944, 8704, 2709a, and 1633c), the recovering efficiencies of using alkali-fusion methods ranged from 95.3 to 98.3% for Iron, and from 86.6 to 88.1% for Nickel within about 2% of relative standard deviation. On the other hand, those using one of the three wet digestion methods ranged from 77.9 to 105.3% for Iron and from 40.1 to 78.5% for Nickel with over 10% of relative standard deviation. Therefore, one may draw the conclusion that the analytical results derived from Iron and Nickel using alkali-fusion methods are fairly reliable due to the recovering efficiencies observed.

• Analytical Science and Technology
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• v.16 no.2
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• pp.152-158
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• 2003

This study was conducted to evaluate two sample digestion procedures and instrumental determination parameters for analysis of lead in bone. Amputated human legs were treated by acid digestion or microwave dissolution prior to spectrometric analysis. Inductively coupled plasma mass spectrometry (ICP-MS) and graphite furnace atomic absorption spectrometry (GF-AAS) were used for determining bone lead levels. Recovery efficiencies using standard reference material from acid digestion measured by ICP-MS were in good agreement with those of the certified value, but in cases of acid digestion by GF-AAS and microwave digestion by both two methods, recovery underestimated and overestimated, respectively. For the bone samples, the lead concentrations obtained by ICP-MS after acid digestionwere in good agreement with those by GF-AAS (correlation coefficient = 0.983), but GF-AAS gave systematically higher values than ICP-MS. While a good agreement between two analytical methods after microwave digestion was also obtained (correlation coefficient = 0.950), bone lead concentrations from microwave were relatively higher than those from acid digestion. In conclusion, the use of the simple nitric acid digestion procedure at an ambient temperature coupled to ICP-MS seems to be efficient for the determination of lead in bone in consideration for both the convenience and validity.

• 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.

• Economic and Environmental Geology
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• v.45 no.6
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• pp.673-684
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• 2012

Quantitative understanding of total carbon, total inorganic carbon and total organic carbon contained in ocean sediments is a basic data for interpretation of oceanic sediment environments. Elemental analyzer(EA) is frequently used for the analysis of carbon contents in inland soils and ocean sediments. Carbon and nitrogen contents of the soil reference material analyzed by an EA were 2.30% and 0.21% with standard deviations of 0.02 and 0.01, respectively. Relative standard deviations were 0.01 and 0.06, respectively, representing a high precision. Regression analysis of TOC and TC analysis results for the samples with TOC of less than 2.0% for the site in Hyung-Do showed a linear relationship with a slope of 0.9743($R^2$=0.9989, n=38), and the results of a relationship regression analysis between total organic carbon contents less than 0.5% and average grain size except for two samples showed a linear relationship with a slope of 0.0444($R^2$=0.6937 n=36). TOC contents of surface sediments were in the ranges of 0.10~1.67%(Average $0.26{\pm}0.37%$) with TOC values of 1.67% at S02 sampling site, 1.13% at S07 sampling site, and less than 1.00% at remaining sites. In the case of PC 01 core sediments, TOC showed the highest value of 0.20% near 70 cm. In the case of PC 02 core sediments, the highest value of 0.24% was indicated near 60 cm. The analysis method of organic carbon obtained from Hyung-Do Intertidal zone sediment sample results may be considered applicable to an organic carbon analysis for ocean sediments and useful for organic carbon analysis experiments of ocean sediments with a reduction in time required for the analysis and a high precision coupled with a high accuracy.

• 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.