• Title/Summary/Keyword: ion detection

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Quantitative determination of inosine 5'-monophosphate dehydrogenase activity in human peripheral blood mononuclear cells by ion-pair reversed-phase high-performance liquid chromatography (이온쌍 역상 HPLC를 이용한 인체 말초혈액단핵구에서 이노신 5'-일인산 탈수소효소 활성의 정량적 측정)

  • Shin, Hye-Jin;Kwon, Soon-Ho;Park, Ji-Myeong;Kwon, Soon-Hyo;Lee, Kyoung-Ryul;Kim, Young-Jin;Lee, Sang-Hoo
    • Analytical Science and Technology
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    • v.23 no.6
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    • pp.531-536
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    • 2010
  • A quantitative analytical method has been established for the measurement of inosine 5'-monophosphate dehydrogenase (IMPDH) activity in human peripheral blood mononuclear cells (PBMCs) by ion-pair reversed-phase high performance liquid chromatography equipped with ultraviolet detection (HPLC/UV). IMPDH is a ${\beta}$-nicotinamide adenine dinucleotide hydrate (NAD+)-dependent dehydrogenase in which the enzyme converts inosine 5'-monophosphate (IMP) into xanthosine 5'-monophosphate (XMP). Its activity was measured by quantifying a HPLC chromatogram corresponding to XMP produced during the incubation of lysed PBMCs with IMP as a substrate and $NAD^+$ as a coenzyme. XMP produced was detected at a wavelength of 260 nm. The mobile phase was composed of a mixture of 37 mM potassium dihydrogen phosphate containing 7 mM tetra-n-butylammonium hydrogen sulfate adjusted to pH 5.5 and methanol (85:15, v/v) with a flow rate of 1 mL/min. The calibration curve was linear ($r^2$=0.999999) in the range of $0.2-50.0\;{\mu}M$ and the limit of quantification (LOQ) was $0.2\;{\mu}M$. The intra- and inter-day precisions were between 0.88-1.47% and 0.85-5.24%, respectively. The intra- and inter-day accuracies were between 98.74-99.99% and 99.95-101.65%, respectively. IMPDH activity in 11 Korean healthy volunteers ranged from 18.29 to 36.60 nmol/h/mg protein (mean = $27.70{\pm}6.28\;nmol/h/mg$ protein).

Optimization of HPLC Method and Clean-up Process for Simultaneous and Systematic Analysis of Synthetic Color Additives in Foods (식품 중 타르색소의 동시분석 및 계통분석을 위한 HPLC 분석조건 및 정제과정 확립)

  • Park, Sung-Kwan;Hong, Yeun;Jung, Yong-Hyun;Lee, Chang-Hee;Yoon, Hae-Jung;Kim, So-Hee;Lee, Jong-Ok
    • Korean Journal of Food Science and Technology
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    • v.33 no.1
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    • pp.33-39
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    • 2001
  • To develop a method for separation process using Sep-pak $C_18$, simultaneous and systematic analysis of 8 permitted and 11 non-permitted synthetic food colors in Korea, optimization of analysis conditions for reverse phase ion-pair high performance liquid chromatography was carried out. For the best result of Sep-pak $C_18$ separation the pH of color standard mixture solution was $5{\sim}6$ and 0.1% HCl-methanol solution were set as eluent. The colors eluated from Sep-pak $C_18$ cartridge were determined and confirmed by high performance liquid chromatography with a photodiode array detector at 420 nm for yellow colors type, at 520 nm for red colors type, at 600 nm for blue and green colors type and at 254 nm for mixed colors. Conditions for HPLC analysis were as follows: column, Symmetry $C_18$ (5 m, 3.9 mm $i.d.{\times}150\;mm$); mobile phase, 0.025 M ammonium acetate (containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (65 : 25 : 10) and 0.025 M ammonium acetate(containing 0.01 M tetrabutylammonium bromide) : acetonitrile : methanol (40 : 50 : 10); flow rate, 1 mL/min. It takes 35 minutes for simultaneaus analysis and 18 minutes for systematic analysis. The detection limits range of each colors were $0.01{\sim}0.05\;{\mu}g/g$.

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Analysis and Uncertainty Estimation of Zearalenone in Cereal-Based Products by LC-MS/MS (LC-MS/MS를 이용한 곡류가공품의 제랄레논 분석과 측정불확도 추정)

  • Choi, Eun Jung;Kang, Sung Tae;Jung, So Young;Shin, Jae Min;Jang, Min Su;Lee, Sang Me;Kim, Jung Hun;Chae, Young Zoo
    • Korean Journal of Food Science and Technology
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    • v.44 no.6
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    • pp.658-665
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    • 2012
  • A survey of zearalenone contamination was conducted on cereal-based products by using an immunoaffinity column with LC-MS/MS. The calibration curve showed good lineality, with correlation coefficients ($R^2$) of 0.999 in the concentration range from 1 to 250 ng/mL. The limits of detection and quantification were approximately $0.3{\mu}g/kg$ and $1.0{\mu}g/kg$, respectively. The recoveries in the barley tea, Misutgaru and snack ranged from 73.6-107.8%. Zearalenone was detected in 10 samples (11.2% incidence). The highest zearalenone contamination level was $29.7{\mu}g/kg$ in the Misutgaru. This survey was conducted with uncertainty of measurement. The expanded uncertainty for zearalenone was estimated to be $44.9{\pm}5.0{\mu}g/kg$ (k=2, 95% confidence level) and $128.7{\pm}7.9{\mu}g/kg$ (k=2, 95% confidence level) for barley tea, $30.7{\pm}5.8{\mu}g/kg$ (k=2, 95% confidence level) and $173.7{\pm}14.9{\mu}g/kg$ (k=2.26, 95% confidence level) for Misutgaru, and $37.2{\pm}7.4{\mu}g/kg$ (k=2.31, 95% confidence level) and $151.0{\pm}10.4{\mu}g/kg$ (k=2, 95% confidence level) snack at the level of $41.7{\mu}g/kg$ and $166.7{\mu}g/kg$, respectively.

The Naturally Occurring Levels of Nitrate and Nitrite in Livestock Products (축산물 중 천연유래 질산염 및 아질산염 함유량 조사)

  • Choi, Jae-Chun;Park, So-Ra;Lim, Ho-Soo;Ko, Kyung-Yuk;Kim, Meehye
    • Journal of Food Hygiene and Safety
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    • v.30 no.3
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    • pp.265-271
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    • 2015
  • This study was done in order to investigate the naturally occurring levels of nitrate and nitrite in livestock products. Total samples of 458 consisting of meats (n = 223), processed meat products (n = 51), raw milks (n = 30), processed milk products (n = 142), eggs (n = 5) and processed egg products (n = 7) were analyzed for contents of nitrate and nitrite by ion chromatography (IC). That methods showed good results in terms of linearity, limit of detection (LOD), limit of quantitation (LOQ), recovery, reproducibility and uncertainty. Nitrate and nitrite were detected in 167 and 40 samples, respectively. The nitrate levels (mg/kg) were not detected (ND)~40.23 for modified milks, ND~37.97 for sauce meats, ND~32.40 for process cheeses, ND~31.50 for processed egg products, ND~27.73 for dry milks, ND~24.76 for sausages, ND~22.45 for bacons, ND~21.55 for natural cheeses, ND~20.82 for hams and fermented milks, ND~13.57 for eggs, ND~12.77 for butters, ND~9.31 for milks and ND~3.88 for meats while the nitrite levels (mg/kg) were ND~17.35 for processed egg products and ND~1.92 for meats. In conclusion, the result of this study of nitrate and nitrite in livestock products could be used as one of scientific base datum to determine whether they are naturally occurring or not, including ingredients and their percentage, manufacturing processes, other papers relating to naturally occurring levels of them, and so on.

A Study of Interference Factor of Analysis Method of Hexavalent Chromium in Soil using UV/VIS Spectrometry and Application of Ion Chromatography (자외선/가시선 분광법을 이용한 토양 중 6가 크롬 분석방법의 방해요인 분석 및 이온크로마토그래피 적용에 관한 연구)

  • Noh, Hoe-Jung;Lee, Myung-Gyu;Lee, Hyeon Seok;Kim, Mira;Kim, Dongho;Kim, Tae Seung
    • Journal of Soil and Groundwater Environment
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    • v.17 no.6
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    • pp.33-42
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    • 2012
  • This study was performed to find the problems according to interference factors (organic matter, pH, Cr, Mn, Fe, clay, and etc.) when we analyzed the hexavalent chromium [Cr(VI)] in soils using UV/VIS spectrometer (US EPA 7196A), attempted to evaluate the domestic applicability of analytical method (US EPA 7199) using IC-UV/VIS spectrometer as alternative method. The recovery rate of certified reference materials was 75.0% (US EPA 7196A) and 101.4% (US EPA 7199) by the analytical methods. As the results of performing QA/QC about US EPA 7199, method detection limit (MDL) and limit of quantification (LOQ) were 0.062 mg/kg, 0.196 mg/kg, respectively. The LOQ of US EPA 7199 was lower than that of the current soil official testing method in Korea (0.5 mg/kg). Cr(VI) contents in 23 soil samples were compared by the analytical methods of EPA 7196A and 7199. Cr(VI) was detected in 13 of 23 soil samples by EPA 7196A, while EPA 7199 was not detected in any soil samples. The Cr(VI) content in 23 soil samples by EPA 7196A was not clearly correlated with Cr, Fe, Mn and clay content in the soil samples. However, the contents of Cr(VI) and organic matter of the soil samples had the highest coefficient of determination ($R^2$) of 0.80. In order to evaluate the correlation between the recovery rates of Cr(VI) and organic matter contents in the soil samples, the recovery rates of 5 soil samples added Cr(VI) standard solution were analyzed by the analytical methods. According to the results, the higher the organic matter contents in soil samples, the lower the recovery rates of Cr(VI) by US EPA 7196, while in case of US EPA 7199, the recovery rates were stable regardless of the organic matter contents.

Silver Contamination in Drinking Water of Gyeongbuk Area in Korea (경북 지역 먹는 물의 은 검출 특성)

  • Lee, Hea Geun;Kim, Jeong Jin;Kim, Young Hun
    • Korean Journal of Mineralogy and Petrology
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    • v.33 no.3
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    • pp.233-242
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    • 2020
  • As studies and developments of nano-material increase, the release of the nano-sized material to water environment increase. Especially, silver nanoparticles have been found as dissolved and particulate state since nano-silver particle have been intensively used in industrial and our living environment due to the anti-bacterial effect of the nano-particles. The silver nano-particles and silver ion gives adverse effect on ecology and US-EPA set a secondary drinking water standards as 0.1 mg/L. Current study focused on the analysis of silver in groundwater, small scale water supply systems in Gyeongbook area. The results have been compared with the secondary drinking water standards and discussed at the point of characteristics of the local area and purpose of use of the water sample. Among the total of 298 samples, 2 samples exceed the secondary drinking water standards of EPA, 0.64% rate. Community drinking water and simplified water service showed relatively high detection rate and groundwater gave relatively higher concentration of silver indicating anthropogenic source and natural source could contribute simultaneously on groundwater.

Surface Modification Using Spiropyran-Derivative and Its Analysis of Surface Potential Induced by UV (스파이로파이란에 의한 표면 개질 및 자외선에 의해 유도된 표면 전위에 대한 분석)

  • Lee, Bong-Soo;Han, Dong-Keun;Son, Tae-Il;Jung, Young-Hwan
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.478-485
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    • 2011
  • Merocyanine derivatives transformed from spiropyran-containing compounds by irradiating the light of ultraviolet (UV) include zwitterion of phenolate anion and amine cation. Complexation of this phenolate anion on merocyaninemodified surface and Ni ion among metal ions led to a change of surface charge and it was measured with kelvin prove force microscopy (KFM). We found that the resultant surface potential decreased linearly as UV-exposed time increased, and finally were saturated. Also it was analyzed through XPS the immobilized amount of Ni ions was increased according to increase of UV-exposed time. It is considered that these properties could be applied for detection and a quantitative control of different metal ions. Further research is to aim construct specific scaffold/matrix which enable high selective, high sensitive and, especially, a quantitative immobilization of metal ions-binding biomaterials such as proteins and cells.

Spectrophotometric Quantitatification of Fe(II) and Fe(III) Ions Using N,N'-bis(4-methoxysalicylidene) phenylendiamine (N,N'-bis(4-methoxysalicylidene) phenylendiamine를 이용한 Fe(II) 및 Fe(III) 이온의 분광학적 분석)

  • Kim, Sun-Deuk;Seol, Jong-Min
    • Journal of the Korean Chemical Society
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    • v.55 no.3
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    • pp.463-471
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    • 2011
  • A novel $N_2O_2$ Schiff base ligand, N,N'-bis(4-methoxysalicylidene)phenylendiamine(4-$CH_3O$-Salphen), has been synthesized. It has been revealed that the compound is very useful for the spectrophotometric quantification of Fe(II) and Fe(III) ions in aqueous solutions, such as mineral water, hot spring water, sea water, and waste water. The optimum conditions for the quantitative analysis are the followings; [4-$CH_3O$-Salphen]=$4.0{\times}10^{-4}\;M$, DMF/$H_2O$=70/30(v/v), pH=3.4~3.8, T= at $55^{\circ}C$, and prereaction time=1.0 hr. The sample of single valence state was prepared by the preliminary oxidation or reduction using $H_2O_2$ ($5.0{\times}10^{-4}\;M$) and $NH_2OH{\cdot}HCl$ ($5.0{\times}10^{-4}\;M$). The quantitative analyses of Fe(II) and Fe(III) ion were performed by measuring the absorbance at 434 nm and 456 nm, respectively. The estimated mean values agreed well with the standard values within the range of 2.00~6.90%. The limit of detection was 27.9 ng/mL for Fe(II) and 55.8 ng/mL for Fe(III).

Effects and Behaviors of Heavy Metals(Cd, Cr, Cu, Pb) in Cement Clinker Reaction (시멘트 클린커 반응에서 중금속(Cd, Cr, Cu, Pb)의 거동과 영향)

  • Hong, Seong-Su;Lee, Taeck-Hong;Lim, Gye-Gyu;Oh, Hea-Kab;Lee, Bong-Han
    • Applied Chemistry for Engineering
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    • v.10 no.5
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    • pp.696-700
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    • 1999
  • The effects and behaviors of heavy metals incoming from industrial by-products were investigated in cement clinker reaction. The raw meal containing 500 ppm of heavy metal ion such as Cu, Cd, Cr, and Pb was calcined at $1450^{\circ}C$ for 30 minutes. Burnability index, fixation concentration of heavy metals in clinker, and apportionment ratio were analyzed. Pb had a minimum fixation concentration of under 5% and Cr had a maximum over 85%. The burnability of Cr containing clinker was lower than that of others as the result of higher value of 3.41% of free lime after calcination at $1450^{\circ}C$. Cu, Cd, and Pb had not any significant effects on the clinker reactitivity. The volatility of heavy metals produced lots of macropores and micropores in clinker and minerals. Cd and Cr were the major apportionments in alite and belite and Cu in interstitial phase. Pb was existed under the detection limit of EDAX analysis due to its higher volatility.

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Determination of Cd(II) after Preconcentration onto Microcrystalline p-Dichlorobenzene Loaded with 2-Mercaptobenzothiazole (2-Mercaptobenzothiazole이 내포된 p-Dichlorobenzene 미세결정으로 예비농축시킨 후 Cd(II) 정량)

  • Yoon, Ju-Im;Choi, Hee-Seon
    • Journal of the Korean Chemical Society
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    • v.53 no.1
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    • pp.27-33
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    • 2009
  • A sensitive technique for the determination of trace Cd(II) in various real samples after preconcentration onto microcrystalline p-dichlorobenzene loaded with 2-mercaptobenzothiazole was developed. Several experimental conditions such as the pH of the sample solution, the amount of chelating agent 2-mercaptobenzothiazole, the amount of adsorbent p-dichlorobenzene-2-MBT, and the flow rate of sample solution were optimized. The interfering effects of various concomitant ions were investigated. Cu(II) interfered with more seriously than any other ions. However, the interference by Cu(II) could be overcome sufficiently by adjusting tartrate ion concentration to be 0.01M or by controlling the amount of 2-mercaptobenzothiazole contained in 0.20 g p-dichlorobenzene to be 0.12 g. The dynamic range, the correlation coefficient ($R^2$) and the detection limit obtained by this proposed technique were $0.5{\sim}30$ ng $mL^{-1}$, 0.9962, and 0.39 ng $mL^{-1}$, respectively. Thus, good results were obtained by the use of p-dichlorobenze as adsorbent matrix. For validating this proposed technique, the aqueous samples(wastewater, stream water, and reservoir water) and the plastic sample were used. Recovery yields of $93{\sim}104$ % were obtained. By F test, these measured data were not different from ICP-MS data at 95 % confidence level. Based on the results from the experiment, it was found that this proposed technique could be applied to the preconcentration and determination of Cd(II) in various real samples.