• Title/Summary/Keyword: SRM analysis

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An analysis of benzoic acid, methyl paraben and butyl paraben in soy sauce using isotope dilution liquid chromatography mass spectrometry (동위원소희석 질량분석법을 이용한 간장 중의 안식향산, 메틸파라벤, 부틸파라벤의 분석)

  • Ahn, Seonghee
    • Analytical Science and Technology
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    • v.31 no.6
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    • pp.225-231
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    • 2018
  • Benzoic acid, methyl paraben, and butyl paraben are preservatives that have been used in pharmaceutical, cosmetic, and food products. However, as their toxicities for human have been reported, many nations and organizations including Korea have established a regulation limit for thier usage of these preservatives in food products. The present study developed the isotope dilution liquid chromatography mass spectrometry method for accurate determination of three target preseratives in soysauce. In this study, the isotope dilution liquid chromatography mass spectrometry method was developed for accurate determination of three target preservatives in soy sauce. LC separation was optimized considering the pKa of benzoic acid which is lower than those of methyl and butyl parabens. A C18 column was used with 5 mM ammonium acetate and methanol as mobile phases. Mass spectrometry was operated in negative mode and selected reaction monitoring mode (SRM). Soy sauce sample was cleaned-up with C18 SPE cartridge for removing matrix inferences and color material. Optimized conditions and the method were validated with soy sauce reference materials for the analysis of food preservatives from Health Science Authority in Singapore. The measured values of benzoic acid, methyl and butyl paraben agreed well with reference values within their uncertainties.

Characteristics of Total Carbon and Total Organic Carbon Using Elemental Analyzer in Hyung-Do Intertidal Zone Sediments (원소분석기를 이용한 형도 퇴적물의 총탄소 및 총유기탄소 특성)

  • Lee, Jun-Ho;Park, Kap-Song;Woo, Han-Jun
    • 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.

Development of a Method for Detecting Iodide and Chloride Ions in Infant Formula using an Ion Selectivity Electrode (이온선택성 전극법을 이용한 조제분유중의 염소 및 요오드 이온함량 분석방법 연구)

  • Ko, Jin-Hyouk;Kwak, Byung-Man;Ahn, Jang-Hyuk;Jeon, Tae-Hong
    • 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.

Accurate determination of chloramphenicol in meat by isotope dilution liquid chromatography mass spectrometry (ID-LC/MS) (동위원소희석 액체크로마토그래피-질량분석법을 이용한 육류 중 클로람페니콜의 정밀한 정량 분석에 관한 연구)

  • Song, Hye-Min;Kim, Byung-Joo;Jeong, Hyuk;Ahn, Seong-Hee
    • 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.

Analysis of Trench Slope Stability in Permafrost Regions According to the Vertical and Horizontal Angle of Slope (동토지반에서 종방향 및 횡방향 사면의 경사에 따른 트렌치 안전성 분석)

  • Kim, Jong-Uk;Kim, Jung-Joo;Jafri, Turab H.;Yoo, Han-Kyu
    • Journal of the Korean Institute of Gas
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    • v.21 no.1
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    • pp.27-33
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    • 2017
  • In this study, the stability of trench slope was analysed in summer and winter seasons for the construction of pipelines in permafrost regions. The construction standards of Korea, Russia and UK were compared for obtaining an optimum trench shape for a pipeline of 30 in. diameter. Using the geotechnical properties of soil in Yakutsk (Russia), the stability of trench slope was analysed using Strength Reduction Method (SRM) according to the horizontal slope angle values of $0^{\circ}$, $10^{\circ}$, $20^{\circ}$ and $30^{\circ}$ and vertical slope angle values of $20^{\circ}$, $30^{\circ}$ and $40^{\circ}$. In both seasons, an increase in the slope angle results in a decrease in the factor of safety. The results show that horizontal slope angle of $30^{\circ}$ was not safe in summer season. At the vertical slope angle of $20^{\circ}$, trench side failure was observed, whereas, ground slope failure was observed at the vertical slope angles of $30^{\circ}$ and $40^{\circ}$. Due to the solidification of pore water at temperatures below $0^{\circ}C$, cementation of soil particles take place. Therefore, the trench slope was found to be stable in the winter season at all vertical and horizontal slop angles, except for special load cases and abrupt temperature changes.

Measurement of heavy metals in antarctic soil at the king sejong station: application of isotope dilution inductively coupled plasma mass spectrometry (동위원소희석 ICP-MS분석법에 의한 남극 세종기지 주변 토양의 중금속 측정)

  • Suh, Jung-Ki;Hwang, Euijin;Min, Hyung Sik
    • Analytical Science and Technology
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    • v.21 no.5
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    • pp.364-374
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    • 2008
  • Antarctic Environmental Monitoring Handbook' was published by COMNAP/SCAR in 2000. The standardized method described in this handbook is recommended for monitoring of antarctic environment. High pressure bomb technique in this guide was used to decompose soil samples. In compliance with this guide book, high pressure bomb technique was applied to decompose the antarctic soil sampled at the King Sejong Station. An Isotope Dilution-Inductively Coupled Plasma-Mass Spectrometry (ID-ICP-MS) was applied to determine mass concentrations of Pb, Cu and Zn in the soil. The accuracy in this method was verified by the analysis of certified reference materials (CRM) of NIST 2702 (marine sediment). The analytical results agreed with certified value within the range from 99.5~100.8%. Matrix separation was necessitated for the determination of Cu and Zn by Chelex 100 ion exchange resin. As a result, the average mass concentrations of Pb, Cu and Zn which are suspected to be caused by anthropogenic pollution were 332.9 mg/kg, 95.6 mg/kg and 115.3 mg/kg, respectively. Those for the metals sampled in the soils of the remote regions from the station were 28.1 mg/kg, 101.8 mg/kg and 115.6 mg/kg, respectively.

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.

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.