• Title/Summary/Keyword: 1M ammonium acetate

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Determination of Glimepiride in Human Plasma by LC-MS/MS

  • Kim, Ho-Hyun;Roh, Hyeong-Jin;Lee, Hee-Joo;Han, Sang-Beom
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.282.1-282.1
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    • 2003
  • This study established a sensitive novel Quantification method for detecting glimepiride in human plasma using LC-MS/MS for pharmacokinetic studies. The mobile phase used after degassing was composed of 10 mM ammonium acetate and acetonitrile (20:80, pH 3.0), with flow rate of 200uL/min. One mL plasma were pipetted into glass tubes and spiked with 0.1 mL of internal standard solution. (omitted)

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Sensitive Determination of Felodipine in Human Plasma by LC-MS/MS

  • Kim, Ho-Hyun;Roh, Hyeon-Jin;Lee, He-Joo;Han, Sang-Beom
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.283.2-283.2
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    • 2003
  • This study established a highly sensitive novel quantification method for detecting felodipine in human plasma using LC-MS/MS. The mobile phase used after degassing was composed of 1 mM ammonium acetate and acetonitrile (20:80, pH 6.0), with flow rate of 200 uL/min. One mL plasma were pipetted into glass tubes and spiked with 0.1 mL of internal standard solution. (omitted)

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A study on simultaneous determination of residual sulfonamides in livestock productions by high performance liquid chromatography (HPLC를 이용한 축산식품중 잔류 설폰아미드제의 동시분석법 연구)

  • 황래홍;김영수;윤은선;김기근;이규학
    • Korean Journal of Veterinary Service
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    • v.18 no.3
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    • pp.13-28
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    • 1995
  • This study was carried out to explore the most sensitive and useful method for simultaneous determination of five sulfa drugs(sulfamethazine, sulfamerazine, sulfamonomethoxine, sulfadimethoxine, sulfaquinoxaline) in livestock productions(pork muscle, bovine muscle, chicken muscle, milk ) by HPLC with UV detector and reverse phase column. The results obtained were as follows:1. For mobile phase acetonitrile-0.01M ammonium acetate (23:77) showed more applicable sensitivity and retention times than acetonitrile-1% acetic acid(23:77). Thus acetonitrile-0.01M ammonium acetate(23:77) selected and applied to the modification test, from which it was found pH 6.75 was the most adequate. 2. Optimal wavelength of UV for SMT(sulfamethazine), SMR(sulfamerazine), SMM(sulfamonomethoxine), SD(sulfadimethoxine), and SQ(sulfaquinoxaline) were 266, 266, 265, 269 and 250nm, respectively, and that for simultaneous application it was 263nm. 3. The average recovery rate by extractant(chloroform, dichloromethane, chlorform+dich-loromethane) in the classic method was not significantly different(p>0.05) but that by chloroform higher than the others. Thus chloroform was found to be adequate as extractant in this classic method. 4. The average recovery rate was 86.5% by the MSPD(matrix solid phase disperse) method, which was significantly higher than that by the classic method(p<0.05). Also the recovery rates by method were significantly different(p<0.05) in accordance with sample and type of drug. The MSPD method was much superior to classic method on clean-up.

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Analysis of Melatonin Content from Domestic Edible Plants (국내산 식용식물체의 멜라토닌 함량 분석)

  • Kim, Seok-Joong
    • Korean Journal of Food Science and Technology
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    • v.34 no.6
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    • pp.1145-1148
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    • 2002
  • Melatonin, which is a hormone secreted from pineal gland of brain and known to prevent oxidative damages of various tissues, was analyzed in 26 domestic edible plants. For the preparation of melatonin fraction, 50% ethanol extract prepared from lyophilized plant powder was filtered and applied on TLC plate. Melatonin position on TLC developed with acetone was identified by fluorescence light and extracted with methanol. This methanolic fraction was injected into HPLC comprising ODS-A column, fluorescence detector, and mobile phase consisting of a mixture (30 : 70, v/v) of 70% ammonium acetate and methanol at a flow rate of 1.0 mL/min. Melatonin was identified at the retention time of 17 min. Results revealed that celery, leek, broccoli, and cauliflower had higher melatonin contents than others.

Easy-to-execute 'One-pot' Synthesis of 1,2,4,5-Tetrazines Catalyzed by Activated Fly Ash (활성화된 비산회 촉매를 이용하여 간단히 수행된 1,2,4,5-Tetrazines의 One-pot 합성)

  • Gopalakrishnan, M.;Thanusu, J.;Kanagarajan, V.
    • Journal of the Korean Chemical Society
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    • v.51 no.6
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    • pp.520-525
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    • 2007
  • Three-component coupling of thiourea/urea, various structurally diverse aromatic aldehydes and ammonium acetate is catalyzed by activated fly ash in dry media under microwave irradiation to give 6-aryl-1,2,4,5-tetrazinan- 3-thiones/ones in good yields. The structure of 6-aryl-1,2,4,5-tetrazinan-3-thiones/ones have been elucidated on the basis of their melting points, elemental analysis, MS, IR, 1H NMR, D2O exchange, 13C NMR and two dimensional NMR spectral studies including Homonuclear Correlation (HOMOCOR) and Heteronuclear Single Quantum Correlation (HSQC) spectra.

Preparation of Zinc Oxide by Hydrothermal Precipitation and Degradation of Tartrazine (수열 합성법에 의한 Zinc Oxide의 제조 및 Tartrazine 분해 특성)

  • Na, Seok-Eun;Jeong, Sang-Gu;Jeong, Ga-Seop;Kim, Si-Young;Ju, Chang-Sik
    • Korean Chemical Engineering Research
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    • v.49 no.6
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    • pp.752-757
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    • 2011
  • The effects of reaction temperature, reactant concentration, pH of solution and mixing order of reactants on the particle shape and size distribution of zinc oxide were investigated in the preparation of zinc oxide from ammonium hydroxide and zinc acetate by the method of aqueous hydrothermal precipitation method, and the photocatalytic ability of zinc oxide synthesized was measured from the degradation of tartrazine under UV irradiation. The average particle size was increased with pH of solution but decreased with zinc acetate concentration and reaction temperature. The optimum condition for the synthesis of minimum sized zinc oxide was pH 11.2, concentration of zinc acetate 0.6 M and reaction temperature $90^{\circ}C$, and its average particle size was 3.133 ${\mu}$m. 97% of tartrazine was degraded by zinc oxide in sixty minutes.

Determination of Chromium(VI) by Differential-Pulse Polarography with a Sodium Borate Supporting Electrolyte

  • Hong, Tae-kee;Czae, Myung-Zoon
    • Bulletin of the Korean Chemical Society
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    • v.9 no.2
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    • pp.77-80
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    • 1988
  • A suituable choice of supporting electrolyte medium for trace level determinations of chromium(VI) by differential pulse polarography is described. A comparative study suggests that sodium borate buffer is superior to ammonium acetate, ammonium tartrate, and especially to NaF which was recently known to be one of the most proper medium for the purpose. With 0.01 M borate, the best combination of high sensitivity, well-defined base line, and freedom from common interferents was attained. With $5.0{\times}10^{-7}$M Cr(VI), tenfold excesses of Cu(II) and Fe(III), and a five hundred-fold excess of $Cl^-$ do not change the peak current by more than about 1%. And the detection limit was $5.0{\times}10^{-8}$M Cr(VI).

A Study on the Analysis of Five Artificial Sweetners in Beverages by HPLC/MS/MS (HPLC/MS/MS를 이용한 음료류 중 인공감미료 동시분석에 관한 연구)

  • Lee, Seong-Bong;Yong, Kum-Chan;Hwang, Sun-Il;Kim, Young-Su;Jung, You-Jung;Seo, Mi-Young;Lee, Chang-Hee;Sung, Jin-Hee;Yoon, Mi-Hye
    • Journal of Food Hygiene and Safety
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    • v.29 no.4
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    • pp.327-333
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    • 2014
  • A method for analysis of five artificial sweetners (sodium saccharin, aspartame, acesulfame-K, sucralose, cyclamate) in beverage samples was developed using high-performance liquid chromatography/triple quadrupole mass spectrometry (HPLC/MS/MS). The method uses a single-step dilution for sample preperation. Seperation was achieved on a $C_{18}$ column ($2.1{\times}150mm$, $3.5{\mu}m$) with A- 2% methanol (1 mM ammonium acetate), B-95% methanol (1 mM ammonium acetate) as mobile phase with gradient mode. The quantitation of target compounds was performed by external calibration in selected reaction monitorning (SRM) mode. The coefficient of determination of calibration curve for sodium saccharin, aspartame, acesulfame-K, sucralose and cyclamate were 0.9957, 0.9991, 0.9943, 0.9982 and 0.9948, respectively. The limits of detection (LODs) and limits of quantitation (LOQs) were in the range of 0.001~0.022 mg/L and 0.004~0.073 mg/L, repectively. Recoveries for beverage samples were in the range of 92.76~113.50% with RSD < 10.91%. The method has applied to the determination of the five sweetners in 102 beverage samples. Three artificial sweetners-aspartame, acesulfame-K, sucralose were detected from 42 samples. Sodium saccharin and cyclamate were not detected in all samples.

A New Method on the Measurement of Catalase Activity of Panax ginseng C.A. Meyer Tissues (인삼조직에서 Catalase Activity측정에 관한 새로운 Method)

  • Yang, Deok-Cho;Chae, Quae;Yoon, Jae-Jun;Lee, Sung-Jong;Lee, Ae-Ra
    • Journal of Ginseng Research
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    • v.9 no.2
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    • pp.154-162
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    • 1985
  • We report a newassay method on the measurement of the catalase activity, whose utilzation value is considered to be remarkable in the field of plant biochemistry. We named this method as a De-Coupling method. The essence of de-coupling method is the separation between the enzyme reaction and the indicator reaction. The optimum condition of the enzyme reaction was found to be following: on addition of 1 ml of substrate (H2O2: 20mM) to the fixture of the crude extract of enzyme (volume: 0.2 ml) and the ammonium phosphate buffer (volume: 1.8 ml; 0.93 M phosphate, 1.6M NHB, 2.5 M methanol, pH 7.0). After 30, 60 and 90 seconds of the enzyme reactions are proceeded, the reactions are terminated by 25% of tai-chloro-acetate (final concentration of 5%), respectively. The precipitated materials by tai-chloro-acetate was removed by the centrifugation (2000g, 10minutes). Formaldehyde produced in the enzymatic reaction was reacted with 2ml of acetylacetone (60mM). The indicator reaction -(HANTSCH REAKT10N)- in which lutidine is formed, was proceeded for 60 minutes at $25^{\circ}C$.

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Synthesis of New 2-Thiouracil-5-Sulphonamide Derivatives with Antibacterial and Antifungal Activity

  • Fathalla O. A.;Awad S. M.;Mohamed M. S.
    • Archives of Pharmacal Research
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    • v.28 no.11
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    • pp.1205-1212
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    • 2005
  • 2-Thiouracil-5-sulphonic acid N-(4-acetylphenyl) Amide (1) was reacted with a series of aromatic aldehydes giving chalcones 2 (Claisen-Schemidt reaction), some of these chalcones were reacted with urea and thiourea giving pyrimidine-2-one and pyrimidine-2 thione derivatives respectively of the type 3a,b and 4a,b. In addition many chalcones were reacted with hydroxylamine hydrochloride giving isoxazoline derivatives 5a,b. They could also reacted with phenylhydrazine to give pyrazoline derivatives 5a,b, chalcones also were reacted withethylcyano acetate and/or malononitryl in pyridine giving pyran derivatives 7a,c and 8a,c. In another pathway chalcones were epoxidised by $H_{2}O_{2}$ giving epoxides 9a,c which in turn were reacted with phenylhydrazine giving 4-hydroxypyrazoline derivatives 10a,c. In another reaction chalcones were reacted with ethylcyanoacetate in presence of amm.acetate giving pyridone derivatives 11a,d which could be prepared also in exellent yield from compound 1 by its reaction with certain aromatic aldehydes and ethylcyanoacetate in presence of ammonium acetate. Finally, compound 1 was reacted with semicarbazide giving semicarbazone intermediate 12 which in turn was reacted with thionyl chloride giving thiadiazole derivative 13. The biological effects of some of the new synthesized compounds were also investigated.