• Korean Journal of Veterinary Service
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• v.29 no.3
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• pp.339-346
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• 2006

Semi-micro-HPLC using a column-switching technique was developed for simultaneous determination of vitamin A and E contents in infant formula. Vitamin A and E were extracted by PDA - HPLC with reversed phase column using organic solvent and their contents in Certified Reference Material (CRM) and infant formula were determined and compared with hydrolysis method and rapid extraction. Developed method has many advantages of simple and rapid sample preparation and simultaneous determination of vitamin A and E by micro-HPLC using reversed phase column.

• Food Science of Animal Resources
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• v.28 no.3
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• pp.301-305
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• 2008

This study was carried out to develop an accurate and rapid analysis method to measure the contents of iodide and chloride in infant formula using an ion selectivity electrode. The infant formula SRM 1846 (Standard Reference Material 1846, NIST, USA) was used as a CRM (Certified reference material). Samples were dissolved in water with 3% acetic acid and filtered through filter paper and adjusted to pH 7.0 with 0.1N NaOH. At pH 7.0, the iodide content of the CRM was $1.04{\pm}0.03\;mg/kg$ compared to the specification of $1.11{\pm}0.1\;mg/kg$ of CRM, and the recovery was $93.7{\pm}2.7%$. The chloride content was $5114.3{\pm}240\;mg/kg$ compared to the specification of $4,920{\pm}300mg/kg$ of CRM, and the recovery was $103.9{\pm}4.9%$. Ion selectivity electrodes could be successful1y used to determine the concentration of iodide and chloride ions in infant formula by a simple and rapid pretreatment of sample matrixes.

• Journal of the Korean Institute of Gas
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• v.22 no.2
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• pp.46-51
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• 2018

Hydrogen sulfide from landfill and sewage treatment plant is a major odor component and causes many civil petitions. Rapidly developing industries release hydrogen sulfide, an odorous gas, to the atmosphere. This study aims to develop a $10{\mu}mol/mol$ concentration level hydrogen sulfide primary standard gas for odor measurement. The hydrogen sulfide gas was prepared at a nominal concentration of $10{\mu}mol/mol$ in nitrogen using the gravimetric method described in ISO 6142. Replicate standard gases were produced in 4 aluminium cylinders, and their concentrations were verified by GC-AED. The uncertainty of production was less than 0.50 %, and the variation of the 4 replicates was 0.22 %. The wall adsorption of hydrogen sulfide in cylinders was 0.10 % at 1500 psi, and the concentration was estimated to be long-term stable for one year. The relative expanded uncertainty of the preparation consistency, adsorption and long-term stability of this hydrogen sulfide standard gas was less than 1.05 % (95 % of confidence level, k=2).

• Analytical Science and Technology
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• v.23 no.3
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• pp.240-246
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• 2010

A technique for the determination of trace Cu(II) in various real samples by FAAS after the column preconcentration onto p-dichlorobenzene-SA adsorbent, which is microcrystalline p-dichlorobenzene loaded with salicylaldoxime (SA) has been developed. Several experimental conditions such as pH of the sample solution, the amount of chelating agent salicylaldoxime, the amount of adsorbent p-dichlorobenzene-SA, and flow rate of sample solution were optimized. The interfering effects of various concomitant ions were investigated. $CN^-$ interfered more seriously than any other ions. However, the interference by $1\;{\mu}g\;mL^{-1}\;CN^-$ could be overcome completely by controlling the concentration of Ni(II) to $20\;{\mu}g\;mL^{-1}$. The linear range, correlation coefficient ($R^2$) and detection limit obtained by this technique were $3.0\sim100\;ng\;mL^{-1}$, 0.9901, and $3.1\;ng\;mL^{-1}$, respectively. For validating this technique, the aqueous samples (wastewater, reservoir water and stream water) and the food samples (orange juice, fresh egg and skim milk) were used. Recovery yields of 93~104% were obtained. These measured mean values were not differents from ICP-MS data at 95% confidence level. The good results were obtained from the experiments using the rice flour certified reference material (CRM) sample. Based on the experimental results, it was found that this technique could be applied to the preconcentration and determination of Cu(II) for various real samples.

• Analytical Science and Technology
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• v.30 no.5
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• pp.226-233
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• 2017

In general, quantitative chemical analysis in various areas including food, the environment, in vitro diagnostics, etc., requires traceability in order to increase the reliability of the measurements. Measurement traceability is a property of an unbroken chain of comparisons relating an instrument's measurements to SI units. Purity analysis is the first process for establishing traceability to SI units in chemical measurements. The purpose of this study is to develop and validate a method of purity assignment for establishing the traceability of $17{\beta}$-estradiol measurements in an in vitro diagnostics field. The establishment of this method is very important as it can be applied to the development of CRM and to the analysis of the purity of other hormones. The method of assignment of the purity of $17{\beta}$-estradiol was developed using the mass balance method and was validated through participation in an International comparison. In the mass balance method, impurities are categorized into four classes as follows: total related structure impurities, water, residual organic solvents, and nonvolatiles/inorganics. In this study, total related structure impurities were characterized by a gas chromatography-flame ionization detector (GC-FID) and a high-performance liquid chromatography-ultraviolet (HPLC-UV) detector, water content was determined by a Karl-Fisher coulometer, and total residual solvents and nonvolatiles/inorganics were checked simultaneously by thermogravimetric analysis (TGA). The purity of the $17{\beta}$-estradiol was 985.6 mg/g and the expanded uncertainty was 2.1 mg/g at 95% confidence. The developed method can be applied to the development of certified reference materials, which play a critical role in traceability.

• Journal of Radiation Protection and Research
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• v.41 no.4
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• pp.359-367
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• 2016

Background: As new legislation has come into force implementing radiation safety management for the use of naturally occurring radioactive materials (NORM), it is necessary to establish a rapid and accurate measurement technique. Measurement of $^{238}U$ and $^{232}Th$ using conventional methods encounter the most significant difficulties for pretreatment (e.g., purification, speciation, and dilution/enrichment) or require time-consuming processes. Therefore, in this study, the applicability of ED-XRF as a non-destructive and rapid screening method was validated for raw materials and by-product samples. Materials and Methods: A series of experiments was conducted to test the applicability for rapid screening of XRF measurement to determine activity of $^{238}U$ and $^{232}Th$ based on certified reference materials (e.g., soil, rock, phosphorus rock, bauxite, zircon, and coal ash) and NORM samples commercially used in Korea. Statistical methods were used to compare the analytical results of ED-XRF to those of certified values of certified reference materials (CRM) and inductively coupled plasma mass spectrometry (ICP-MS). Results and Discussion: Results of the XRF measurement for $^{238}U$ and $^{232}Th$ showed under 20% relative error and standard deviation. The results of the U-test were statistically significant except for the case of U in coal fly ash samples. In addition, analytical results of $^{238}U$ and $^{232}Th$ in the raw material and by-product samples using XRF and the analytical results of those using ICP-MS ($R^2{\geq}0.95$) were consistent with each other. Thus, the analytical results rapidly derived using ED-XRF were fairly reliable. Conclusion: Based on the validation results, it can be concluded that the ED-XRF analysis may be applied to rapid screening of radioactivities ($^{238}U$ and $^{232}Th$) in NORM samples.

• Mass Spectrometry Letters
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• v.3 no.2
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• pp.58-61
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• 2012

A method based on flow injection-isotope dilution-cold vapor-inductively coupled plasma mass spectrometry (FI-IDCV-ICP/MS) has been applied to determine trace level of mercury in fly ash. $^{200}Hg$ isotopic spike was added to 0.25 g of BCR176R fly ash and then decomposed by microwave digestion procedure with acid mixture A (8 mL $HNO_3$ + 2 mL HCl + 2 mL HF) and acid mixture B (8 mL $HNO_3$ + 2 mL $HClO_4$ + 2 mL HF) for applying IDMS. Mercury cold vapor was generated by using reductant solution of 0.2% (w/w) $NaBH_4$ and 0.05% (w/w) NaOH. The measurements of n($^{200}Hg$)/n($^{202}Hg$) isotope ratio was made using a quadrupole ICP/MS system. The accuracy in this method was verified by the analysis of certified reference material (CRM) of fly ash (BCR 176R). The indicative value of Hg in BCR 176R fly ash was $1.60{\pm}0.23$ mg/kg (k = 2). The determined values of Hg in BCR 176R fly ash by the method of FI-CV-ID-ICP/MS described in this paper were $1.60{\pm}0.24$ mg/kg (k = 3.18) and the analysis results were in well agreement with the indicative value within the range of uncertainty.

• Korean Journal of Veterinary Research
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• v.52 no.2
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• pp.69-74
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• 2012

The analytical method of trace toxic metals in livestock products was confirmed and validated through certified reference material (CRM) and the international proficiency tests. There are some difficulties to determine low levels of toxic metals in livestock products because of interferences due to the matrix. The recoveries of CRM (NIST 1577c) ranged from 73.9 to 119% for lead and from 86.4 to 111% for cadmium in bovine liver. The international proficiency tests were carried out with the milk powder and cocoa powder samples including metals provided by Food Analysis Performance Assessment Scheme (FAPAS$^{(R)}$, UK). The test samples were prepared by microwave digestion using solution of $HNO_3:H_2O_2:H_2O$ (v/v/v = 5 : 2 : 4) and analyzed by ICP/MS. The analytical result of cadmium in milk powder was $121{\mu}g/kg$ with -0.3 of the z-score compared to the assigned value of $131{\mu}g/kg$ by FAPAS$^{(R)}$. The analytical results of lead and cadmium in cocoa powder were $29.2{\mu}g/kg$ and $97.6{\mu}g/kg$, respectively, which satisfied the assigned values of $34.2{\mu}g/kg$ for lead and $126{\mu}g/kg$ for cadmium by FAPAS$^{(R)}$. It is verified that the analytical method is accurate and reliable to determine trace lead and cadmium in livestock products by microwave digestion and ICP/MS.

• Korean Journal of Agricultural Science
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• v.46 no.2
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• pp.315-322
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• 2019

In this study, the contents of ${\beta}$-carotene and cholesterol were evaluated in various types of agricultural and processed foods (vegetables, legume products, dairy products, and eggs). Certified reference material (CRM) with an assigned value was used for the validation of the ${\beta}$-carotene and cholesterol analytical methods. High recoveries (accuracy) of ${\beta}$-carotene (96%) and cholesterol (97%) were obtained from the quantitative analysis of the CRM, with a relative standard deviation (%) of 1.86 and 3.35% for the ${\beta}$-carotene and cholesterol, respectively. Vegetables contained relatively high concentrations of ${\beta}$-carotene (raw Toona sinensis, $1650.97{\mu}g/100g$, a raw small onion, $879.09{\mu}g/100g$, and a raw lettuce stem, $591.89{\mu}g/100g$). The ${\beta}$-carotene values in dried chickpeas ($22.94{\mu}g/100g$) and dried brown lentils ($21.98{\mu}g/100g$) were similar. The highest ${\beta}$-carotene value among the analyzed dairy products was found in banana milk ($234.21{\mu}g/100g$) while other flavored products (strawberry milk and chocolate milk) did not contain any ${\beta}$-carotene. Furthermore, ${\beta}$-carotene was not detected in goat milk and high calcium milk in this study. With regard to cholesterol among the analyzed samples, the highest cholesterol value was found in egg yolk (629.30 mg/100 g), and cooking methods (boiling and frying) had little effect on the cholesterol levels of eggs. In addition, the cholesterol content in vanilla ice cream was 28.77 mg/100 g which was the highest value among the analyzed dairy products.

• Mass Spectrometry Letters
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• v.3 no.2
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• pp.54-57
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• 2012

Mass spectrometric analysis was carried out using multicollector inductively coupled plasma mass spectrometry (MC-ICP-MS) for the precise and accurate determination of the isotope ratios of ultratrace levels of uranium dissolved in 3% $HNO_3$. We used the certified reference material (CRM) 112-A at a trace level of 100 pg/mL for the uranium isotopic measurement. Multiple collectors were utilized for the simultaneous measurement of uranium isotopes to reduce the signal uncertainty due to variations in the ion beam intensity over time. Mass bias correction was applied to the measured U isotopes to improve the precision and accuracy. Furthermore, elemental standard solution with certified values of platinum, iridium, gold, and thallium dissolved in 3% $HNO_3$ were analyzed to investigate the formation rates of the polyatomic ions of $Ir^{40}$ $Ar^+$, $Pt^{40}$ $Ar^+$, $Tl^{40}$ $Ar^+$, $Au^{40}$ $Ar^+$ for the concentration range of 50-400 pg/mL. Those polyatomic ions have mass-to-charge ratios in the 230-245 m/z region that it would contribute to the increase of background intensity of uranium, thorium, plutonium, and americium isotopes. The effect of the polyatomic ion interference on uranium isotope measurement has been estimated.