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      • SCOPUSKCI등재

        Simultaneous Determination of Statins in Human Urine by Dilute-and-Shoot-Liquid Chromatography-Mass Spectrometry

        Jang, Haejong,Mai, Xuan-Lan,Lee, Gunhee,Ahn, Jae Hyoung,Rhee, Jongsook,Truong, Quoc-Ky,Vinh, Dinh,Hong, Jongki,Kim, Kyeong Ho Korean Society for Mass Spectrometry 2018 Mass spectrometry letters Vol.9 No.4

        An innovative, simple, and rapid assay method based on liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) was developed and validated for the simultaneous determination of eight statin drugs in human urine. A simple sample clean-up procedure using the "dilute and shoot" (DAS) approach enabled a fast and reliable analysis. The influence of the dilution factor was investigated to ensure detectability and reduce the matrix effect. Chromatographic separation was performed on a Phenomenex Kinetex C18 column ($50{\times}3.0mm$ i.d., $2.6{\mu}m$) using an elution gradient of mobile phase A composed of 0.1% acetic acid, and mobile phase B composed of acetonitrile, at a flow rate of 0.35 mL/min. Quantitation was performed on a triple quadrupole mass spectrometer operated in multiple reaction monitoring (MRM) mode using electrospray ionization in positive ion mode. The total chromatographic run time was 15 min. The method was validated for selectivity, sensitivity, recovery, linearity, accuracy, precision, and stability. The present method was successfully applied to the analysis of Rosuvastatin in urine samples after oral administration to healthy human subjects.

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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 Korean Society for Mass Spectrometry 2014 Mass spectrometry letters Vol.5 No.2

        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.

      • SCOPUSKCI등재

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

        ( Yeoun Hur ),( Sookil Tae ),( Yun Joo Koh ),( Sung Hyun Hong ),( Young Ho Yoon ),( Haejong Jang ),( Sooji Kim ),( Kyeong Ho Kim ),( Seung Woo Kang ),( Youngshin Lee ),( Sang Beom Han ) 한국질량분석학회 2014 Mass spectrometry letters Vol.5 No.2

        A specific and sensitive liquid chromatography-electrospray ionization tandem mass spectrometry method (LC-ESIMS/ 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 (150 mm × 2.0 mm, 4 μm) 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 μL/min. Porphyrins and the internal standard (IS), coproporphyrin I-15N4, 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.

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