• Title/Summary/Keyword: carboxylic acid

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Simultaneous GC/MS Analyses of Organic acids and Amino acids in Urine using TMS-TFA derivative (TMS-TFA 유도체화를 이용한 소변여지 중 유기산과 아미노산의 GC/MS 동시분석)

  • Yoon, Hye-Ran
    • Analytical Science and Technology
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    • v.19 no.1
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    • pp.107-114
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    • 2006
  • Early diagnosis and medical intervention are critical for the treatment of patients with metabolic disorders. A rapid analytical method was developed for simultaneous quantification of organic acids and amino acids in urine without labor-intensive pre-extraction procedure showing high sensitivity and specificity. A new method consisted of simple two-step trimethylsilyl (TMS)-trifluoroacetyl (TFA) derivatization using GC/MS-selective ion monitoring (SIM). Filter paper urine specimens were dried under nitrogen after being fortified with internal standard (tropate) in a mixture of distilled water and methanol. Methyl orange was added to the residue as indicator reagent. Silyl derivative of carboxylic functional group was followed by trifluoroacetyl derivative for amino functional group. N-methyl-N-(trimethylsilyl-trifluoroacetamide) and N-methyl-bistrifluoroacetamide were consecutively added and heated for 15-20 min at $65^{\circ}C-70^{\circ}C$, for TMS-TFA derivative, respectively. This reactant was analyzed by GC/MS-SIM. Linear dynamic range showed 0.001-50 mg with the detection limit of (S/N=3) 10-200 ng, and the quantification limit of 80-900 ng in urine. Correlation coefficient of regression line was 0.994-0.998. When the method was applied to the patients 'urine, it clearly differentiated the normal from the patient with metabolic disorder. The study showed that the developed method could be the method of choices in rapid and sensitive screening for organic aciduria and amino acidopathy.

The Molecular Weight Dependance of Paramagnetic Gd-chelates on T1 and T2 Relaxation Times (상자성 복합체의 분자량에 따른 T1 및 T2 자기이완시간에 관한 연구)

  • Kim In-Sung;Lee Young-Ju;Kim Ju-Hyun;Sujit Dutta;Kim Suk-Kyung;Kim Tae-Jeong;Kang Duk-Sik;Chang Yong-Min
    • Progress in Medical Physics
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    • v.17 no.2
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    • pp.61-66
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    • 2006
  • To evaluate the T1, T2 magnetic relaxation properties of water molecule according to molecular weight of paramagnetic complex. 4-aminomethyicyclohexane carboxylic acid (0.63 g, 4 mmol) was mixed with the suspension solution of DMF (15 ml) and DTPA-bis-anhydride (0.71 g, 2 mmol) to synthesize the ligand. The ligand was then mixed with $Gd_2O_3$ (0.18 g, 0.5 mmol) to synthesize Gd-chelate. For the measurement of magnetic relaxivity of paramagnetic compounds, the compounds were diluted to 1 mM and then the relaxation times were measured at 1.57 (64 MHz). Inversion-recovery pulse sequence was employed for T1 relaxation measurement and CPMG (Carr-Purcell-Meiboon-Gill) pulse sequence was employed for T2 relaxation measurement. In case of inversion recovery sequence, total 35 images with different inversion time(T1)s ranging from 50 msec to 1,750 msec. To estimate the relaxation times, the signal intensity of each sample was measured using region of Interest (ROI) and then fitted by non-linear least square method to yield T1, T2 relaxation times and also R1 and R2. Compared to T1=($205.1{\pm}2.57$) msec and T2=($209.4{\pm}4.28$) msec of Omniscan (Gadodiamide), which is commercially available paramagnetic MR agent, T1 and T2 values of new paramagnetic complexes were reduced along with their molecular weight. That is, T1 value was ranged from $(96.35{\pm}2.04)\;to\;(79.38{\pm}1.55)$ msec and T2 value was ranged from $(91.02{\pm}2.08)\;to\;(76.66{\pm}1.84)$ msec. Among new paramagnetic complexes, there is a tendency that the R1 and R2 increase as the molecular weight is increases. As molecular weight of paramagnetic complex increases, T1 and T2 relaxation times reduce and thus the increase of relaxivity (R1 and R2) Is proportional to molecular weight.

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Acetolactate Synthase Activity Inhibition and Herbicidal Activity of Sulfonylurea and Imidazolinone Herbicides (Sulfonylurea 및 imidazolinone계 제초제(除草劑)의 살초작용(殺草作用)과 acetolactate synthase 활성(活性) 억제작용(抑制作用))

  • Hwang, I.T.;Hong, K.S.;Cho, K.Y.
    • Korean Journal of Weed Science
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    • v.15 no.1
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    • pp.54-62
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    • 1995
  • Acetolactate synthase activity inhibition and herbicidal activities were investigated with 2 sulfonylureas [chlorsulfuron{2-chloro-N-{{(4-methoxy-6-methyl-1,3,5-triazin-2-yl) amino} carboxyl} benzenesulfonamide}, metsulfuron-methyl{methyl-2{{{{(4-methoxy-6-methyl-1,3,5-triazin-2-yl)amino}carbonyl}amino}sulfonyl}benzoic acid}, and 2 imidazoli-nones [imazethapyr{2-{4,5-dihydro-4-methyl-4-(1-methyl)-5-oxo-1H-imidazol-2-yl}-5-ethyl-3-pyridinecarboxylicacid}, imazaquin{2-{4,5-dihydro-4-methyl-4-(1-methyl)-5-oxo-1H-imidazol-2-yl}-3-quinoline carboxylic acid} herbicides. A broad weeding spectrum was observed with the treated herbicides at low application rates. Both corn(Zea mays L.) and sorghum(Sorghum bicolor Moench) were very sensitive to the two herbicide groups. Although legumes, such as soybean(Glycine max Merr.), clover(Trifolium repense L.), and indian jointvetch(Aeschnomene indica L.) were sensitive to the sulfonylureas, they were tolerant to the imidazolinones. On the contrary, wheat(Triticum aestivum L.) and barley(Hoderum sativum Jess.) showed the reverse responses of the legumes to the two herbicide groups. Quackgrass(Agropyron repens(L.) P. Beauv.). however, was commonly tolerant to the two herbicide groups. Degrees of crop injury and acetolactate synthase inhibition also varied with the crops examined. The 50% inhibition concentrations of sulfonylureas on acetolactate synthase in vitro activity($IC_{50}$) from corn, wheat, and soybean did not relate to the greenhouse herbicidal activities ($GI_{50}$). With chlorsulfuron, for example, wheat had more than 100 times higher $GI_{50}$ than corn and soybean, but the $IC_{50}$ was 4 to 10 times lower. Similar observation was made with metsulfuron-methyl. However, closer relationships between $IC_{50}$ and $GI_{50}$ were found with the imidazolinones. When imazethapyr was applied, the order of $GI_{50}$ values against com, wheat, and soybean was the same as that of $IC_{50}$.

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Quantitative Microbial Risk Assessment Model for Staphylococcus aureus in Kimbab (김밥에서의 Staphylococcus aureus에 대한 정량적 미생물위해평가 모델 개발)

  • Bahk, Gyung-Jin;Oh, Deog-Hwan;Ha, Sang-Do;Park, Ki-Hwan;Joung, Myung-Sub;Chun, Suk-Jo;Park, Jong-Seok;Woo, Gun-Jo;Hong, Chong-Hae
    • Korean Journal of Food Science and Technology
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    • v.37 no.3
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    • pp.484-491
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    • 2005
  • Quantitative microbial risk assessment (QMRA) analyzes potential hazard of microorganisms on public health and offers structured approach to assess risks associated with microorganisms in foods. This paper addresses specific risk management questions associated with Staphylococcus aureus in kimbab and improvement and dissemination of QMRA methodology, QMRA model was developed by constructing four nodes from retail to table pathway. Predictive microbial growth model and survey data were combined with probabilistic modeling to simulate levels of S. aureus in kimbab at time of consumption, Due to lack of dose-response models, final level of S. aureus in kimbeb was used as proxy for potential hazard level, based on which possibility of contamination over this level and consumption level of S. aureus through kimbab were estimated as 30.7% and 3.67 log cfu/g, respectively. Regression sensitivity results showed time-temperature during storage at selling was the most significant factor. These results suggested temperature control under $10^{\circ}C$ was critical control point for kimbab production to prevent growth of S. aureus and showed QMRA was useful for evaluation of factors influencing potential risk and could be applied directly to risk management.

A Study on the Protective Effects of Glutathione on Cytotoxicity of Mercury and Cadmium (수은 및 카드뮴의 세포독성에 대한 Glutathione의 역할에 관한 연구)

  • Jeong, Jae-Ho;Kim, Jun-Youn;Koh, Dai-Ha
    • Journal of Preventive Medicine and Public Health
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    • v.32 no.2
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    • pp.170-176
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    • 1999
  • Objectives: To evaluate the protective effects of glutathione (GSH) on the cytotoxicity of mercurial compounds$(CM_3HgCl,\;HgCl_2)$ or cadmium chloride$(CdCl_2)$ in EMT-6 cells. Methods: The compounds investigated were $CH_3HgCl,\;HgCl_2,\;CdCl_2$, GSH, buthionine Sulfoximine(BSO), L-2-oxothiazolidine-4-carboxylic acid(OTC). Cytotoxicity analysis consist of nitric oxide(NO) production, ATP production and cell viability. Results: Mercurial compounds and cadmium chloride significantly decreased cell viability and the synthesis of NO and cellular ATP in EMT-6 cells. GSH was not toxic at concentrations of 0-1.6 mM. In the presence of GSH, mercurial compounds and cadmium did not decrease the production of ATP and nitrite in EMT-6 cells. The protective effects of GSH against the cytotoxicity of mercurial compounds and cadmium depended on the concentration of added GSH to the culture medium for EMT-6 cells. We evaluated the effects of intracellular GSH level on mercury- or cadmium-induced cytotoxicity by the pretreatment experiments. Pretreatment of GSH was not changed ${NO_2}^-$ and ATP production, and pretreatment of BSO was decreased in dose and time-dependent manner. Pretreatment of OTC was increased ${NO_2}^-$ and ATP production in dose- and tine-dependent manner. Because intracellular GSH level was increased by OTC pretreatment, the protective effect on mercury- and cadmium-induced cytotoxicity was increased. Conclusions: These results indicated that sulfhydryl compounds had the protective effects against mercury-induced cytotoxicity by the intracellular GSH levels.

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