• Title/Summary/Keyword: $CO_2$-Acetonitrile

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Determination of Eupatilin in Human Plasma by Liquid Chromatography/Electrospray Ionization Tandem Mass Spectrometry

  • Lee, Hye-Won;Ji, Hye-Young;Kim, Hui-Hyun;Kim, Sook-Jin;Kim, Soon-Hoe;Kim, Won-Bae;Lee, Hye-Suk
    • Proceedings of the PSK Conference
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    • 2003.10b
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    • pp.223.2-223.2
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    • 2003
  • A rapid, sensitive and selective liquid chromatography-tandem mass spectrometric (LC/MS/MS) method for the determination of eupatilin in human plasma was developed. Eupatilin and internal standard, (S)-[N-3-(4-(2-(1-methyl-5-tetrazolyl)-pyridine-5-y1)- 3-fluorophenyl)-2-oxo-5-oxazolidinyl]methyl acetamide (DA-7867) were extracted from human plasma by liquid-liquid extraction and analyzed on a phenyl-hexyl column with the mobile phase of acetonitrile-ammonium formate (10 mM, pH 3.0) (60:40, v/v). (omitted)

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Solvent Effect on the Aquation of $trans-[Cr(en)_2Br_2]^+$ Ion and its Mechanism ($trans-[Cr(en)_2Br_2]^+$ 착이온의 수화반응에 미치는 용매효과와 그 반응메카니즘)

  • Jeong, Jong Jae;Lee, Seong Ho;Baek, Seong O
    • Journal of the Korean Chemical Society
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    • v.34 no.2
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    • pp.123-129
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    • 1990
  • The rate constants for the solvolysis of $trans-[Cr(en)_2Br_2]^+$ ion were determined by the spectrophotometric method in methanol-, ethanol-, acetone-, and acetonitrile-water mixtures, at 20, 25, 30, and 35$^{\circ}C$, respectively. The rate constants increased with increasing co-solvent compositions. The rate constant did not show any relation with the reciprocal of dielectric constant of the solvent-mixtures. The m values of Grunwald-Winstein equation for methanol-, ethanol-, acetonitrile-, and acetone-water mixtures are 0.109, 0.103, 0.101, and 0.095, respectively. A free energy cycle for the process from the initial state to the transition state in water and water + co-solvent mixtures shows that the change in solvation at the transition state has a dominant effect on the rate. From the above results, it is believed that the mechanism for the aquation of this complex is the Id mechanism.

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MEASUREMENT OF SYNTHESIS RATE OF LONG-CHAIN ACYL-COENZYME A ESTER IN BOVINE LIVER BY HIGH-PERFORMANCE LIQUID CHROMATOGRAPHY

  • Mitsuhashi, T.;Mitsumoto, M.;Yamashita, Y.;Ozawa, S.
    • Asian-Australasian Journal of Animal Sciences
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    • v.1 no.2
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    • pp.99-106
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    • 1988
  • A high performance liquid chromatographic procedure is described for the direct determination of the picomole amount of palmitoyl-Coenzyme A and stearoyl-Coenzyme A, using a stainless steel column packed with C-18 derivatized porous silica ($5{\mu}m$), an isocratic elution with a mixture of 33 mM $KH_2PO_4$/acetonitrile as a mobile phase and a UV detector. The long-chain acyl-Coenzyme A esters were determined in incubated microsomal fractions of a bovine liver to demonstrate the utility of this method for monitoring acyl-CoA synthesis in biological samples. The reaction rate of palmitate was higher than that of stearate. After a 60 minute incubation period, the generated amount of palmitoyl-Coenzyme A and stearoyl-Coenzyme A were approximately 70 and 20 n mol/mg micresomal protein, respectively. The advantage of this method are in that no decomposition of the CoA esters is involved, while the constituent molecular species is detected.

Decomposition Characteristics of Bisphenol A by a Catalytic Ozonation Process (오존촉매산화공정에 의한 비스페놀 A의 분해특성)

  • Choi, Jae Won;Lee, Hak Sung
    • Applied Chemistry for Engineering
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    • v.26 no.4
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    • pp.463-469
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    • 2015
  • Bisphenol A (BPA) in aqueous solution was measured using HPLC technique, which was established by acetonitrile analysis and KDP solution analysis methods. In these experiments the decomposition characteristics of BPA were compared using the ozone alone, ozone/pH 10, and ozone/hydrogen peroxide processes. About 70% of 10 mg/L of BPA was removed during 60 min by the ozone alone process, while 10 mg/L of BPA was completely removed by the ozone/pH 10 and ozone/hydrogen peroxide processes in 40 min and 60 min, respectively. The final decomposition efficiency drawn from results of TOC and HPLC analyses showed that the ozone/hydrogen peroxide process was the best among them, whereas the concentrations of TOC and reaction intermediates when using the ozone/pH 10 process were higher than those of the ozone alone process after 60 min of reaction. The ozone/hydrogen peroxide process was the most efficient among them when oxidizing organic carbons in water to $CO_2$ and $H_2O$.

Determination of meloxicam in human plasma by semi-micro high-performance liqiud chromatography.

  • Park, Chang-Hun;Kim, Ho-Hyun;Lee, Hee-Joo;Beom, Han-Sang
    • Proceedings of the PSK Conference
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    • 2003.04a
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    • pp.276.1-276.1
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    • 2003
  • This study describes a simple and sensitive semi-micro HPLC method with UV detection and direct deproteinization. The plasma protein was precipitated using perchloric acid (60%) and the supernatant was directly injected onto the semi-micro HPLC system. The separation was achieved on a C18 (25 mm ${\times}$ 2.0 mm I.D) analytical column with a mobile phase of sodium acetate buffer (pH 3.5, 50 mmol) - acetonitrile (60:40, V/V). (omitted)

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Simultaneous Determination of Five Porphyrins in Human Urine and Plasma Using High Performance Liquid Chromatography-Tandem Mass Spectrometry

  • Hur, Yeoun;Tae, Sookil;Koh, Yun-Joo;Hong, Sung-Hyun;Yoon, Young Ho;Jang, Haejong;Kim, Sooji;Kim, Kyeong Ho;Kang, Seung Woo;Lee, Youngshin;Han, Sang Beom
    • Mass Spectrometry Letters
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    • v.5 no.2
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    • pp.42-48
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    • 2014
  • A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method (LC-ESI-MS/MS) was developed and validated for the simultaneous quantification of porphyrins (coproporphyrin, pentacarboxylporphyrin, hexacarboxylporphyrin, heptacarboxylporphyrin, and uroporphyrin) in human plasma and urine. Acidified plasma samples and urine samples were prepared by using liquid-liquid extraction using ethyl acetate and protein precipitation with acetonitrile, respectively. The separation was achieved onto a Synergi Fusion RP column ($150mm{\times}2.0mm$, $4{\mu}m$) with a gradient elution of mobile phase A (0.1% formic acid in 2 mmol/L ammonium acetate, v/v) and mobile phase B (20% methanol in acetonitrile, v/v) at a flow rate of $450{\mu}L$/min. Porphyrins and the internal standard (IS), coproporphyrin I-$^{15}N_4$, were detected by a tandem mass spectrometer equipped with an electrospray ion source operating in positive ion mode. Multiple reaction monitoring (MRM) transitions of the protonated precursor ions and the related product ions were optimized to increase selectivity and sensitivity. The proposed method was validated by assessing selectivity, linearity, limit of quantification (LOQ), precision, accuracy, recovery, and stability. The calibration curves were obtained in the range of 0.1-100 nmol/L and the LOQs were estimated as 0.1 nmol/L for all porphyrins. Results obtained from the validation study of porphyrins showed good accuracy, precision, recovery, and stability. Finally, the proposed method was successfully applied to clinical studies on the autism spectrum disorder (ASD) diagnosis of 203 Korean children.

Nucleophilic Displacement of Sulfur Center, Part Ⅵ - Halide Exchange Kinetics of Methanesulfonyl Chloride in Acetone, Acetonirile and Methanol

  • Lee, Ikchoon;Yie, Jae-Eui
    • Nuclear Engineering and Technology
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    • v.6 no.1
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    • pp.23-26
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    • 1974
  • The rates and activation parameters for the halide exchange reactions of methanesulfonyl chloride in dry acetone, acetonitrile, and methanol have been determined. It was found that nucleophilic order is Cl->Br->I-. The rate of chloride exchange with methanesulfonyl chloride decreases in the order of solvent; ($CH_3$)$_2$CO>$CH_3$CN》MeOH. Results are intrpreted in terms of easiness of the initial state desolvation and solvation stabilization of the transition state.

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Syntheses and Reactions of Iridium Complexes Containing Mixed Phosphine-Olefin Ligand: (3-(Diphenylphosphino)propyl)(3-butenyl)phenylphosphine

  • Young-ae W. Park;Devon W. Meek
    • Bulletin of the Korean Chemical Society
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    • v.16 no.6
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    • pp.524-528
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    • 1995
  • The reaction of [IrCl(cod)]2 with ppol ligand, Ph2PCH2CH2CH2P(Ph)CH2CH2CH=CH2, in ethanol gives an iridium complex, whose structure is converted from an ionic form, [Ir(cod)(ppol)]Cl·2C2H5OH (1),in polar solvents (ethanol, methanol and acetonitrile), to a molecular form, [IrCl(cod)(ppol)], in non-polar solvents (benzene and toluene). The cationic complexes, [Ir(cod)(ppol)]AsF6·1/2C2H5OH and [Ir(cod)(ppol)]PF6·1/2CH3CN, were prepared to compare with the ionic form by 31P NMR spectroscopy. When carbon monoxide is introduced to 1, cod is replaced by CO to give the 5-coordinated complex, [IrCl(CO)(ppol)]. Hydrogenation of 1-octene was not successful in the presence of 1. In order to verify the reason for 1 not behaving as a good catalyst for hydrogenation, electrophilic reactions with HCl, I2 and HBF4·etherate were performed, which yielded the oxidative addition product, [IrHCl2(ppol)], the substitution product, [IrI(cod)(ppol)], and another cationic product, [Ir(cod)(ppol)]BF4, respectively. Thus, the iridium complex is not sufficiently basic to activate hydrogen atoms or the olefin of the ppol ligand.

Changes of Tobacco Smoke Components by Adding Oriental, Reconstituted, and Expanded tobacco leaves (오리엔트엽, 판상엽, 팽화엽 첨가에 따른 담배 연기성분 변화)

  • 황건중;이문수;나도영;이윤환
    • Journal of the Korean Society of Tobacco Science
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    • v.24 no.2
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    • pp.113-120
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    • 2002
  • This study was conducted to determine the smoke component changes by adding oriental, reconstituted, and expanded tobacco leaves. 7 different cigarette brands which were mixed with flue-cured, burley, oriental, reconstituted and expanded tobacco leaves were used for this study. 64 kinds of smoke components which were 6 of general components, 34 of semi-volatile and volatile components, 9 of acid components, and 15 of phenolic components were analyzed. All smoke components of mainstream smoke were changed by the different branding. As Tar, nicotine, ammonia, pH, all of acid compounds(except lacatic and glycolic acid) were decreased; HCN, levoglucosame, 4-vinyl phenol, 4-vinyl catechol, quinic acid-r-lactone, acetaldehyde, 2,3-butadiene, stylene were increased by adding oriental tobacco leaves. When the reconstituted tobaccos were added to 20%, the concentration of nicotine, all of acid compounds(except lactic. glycolic, palmitic acid) and all of phenol compounds were reduced; the concentration of ammonia, HNC, CO, aeconitrile, benzene, 2-butanone, moth-acrolene, butyronitrile, stylene, o-xylene were increased. As decreasing ammonia, pH, nicotine, all of acid compounds, all of phenol compounds, Isoprene, acetonitrile, 2-methyl-2-butene, 1,3-pentadiene, 2-nlethyl furane, ethylene cyclopentanone, ethyl bezene; increasing CO concentration were followed by adding expanded tobacco leaves.

Resolution of Salbutamol Enantiomers in Human Urine by Reversed-Phase High Performance Liquid Chromatography after Derivatization with 2,3,4,6-Tetra-O-acetyl-${\beta}$-D-glucopyranosyl Isothiocyanate

  • Kim, Kyeong-Ho;Kim, Tae-Kyun
    • Archives of Pharmacal Research
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    • v.21 no.2
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    • pp.217-222
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    • 1998
  • A stereospecific HPLC method has been developed for the resolution of the enantiomers of salbutamol in human urine. After solid-phase extraction and derivatization with 2,3,4,6-tetra-O-acetyl-$\beta$-D-glucopyranosyl isothiocyanate, the diastereomeric derivatives were resolved (Rs=1.83) on $5{\mu}m$ octadecylsilan column using 35% acetonitrile in 0.05M ammonium acetate buffer (pH=6) as a mobile phase with electrochemical detection. The diastereomeric derivatives were formed within 30 min. The detection limit of each enantiomer was 20 ng/ml (S/N=3).

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