A selective precolumn derivatization liquid chromatography–tandem mass spectrometric (LC–MS/MS) method for the determination of glucosamine in human plasma and urine has been developed and validated. Glucosamine was...A selective precolumn derivatization liquid chromatography–tandem mass spectrometric (LC–MS/MS) method for the determination of glucosamine in human plasma and urine has been developed and validated. Glucosamine was derivatized by o-phthalaldehyde/3-mercaptopropionic acid. Chromatographic separation was performed on a Phenomenex ODS column (150 mm 4.6 mm, 5 mm) using linear gradient elution by a mobile phase consisting of methanol (A), and an aqueous solution containing 0.2% ammonium acetate and 0.1% formic acid (B) at a flow rate of 1 mL/min. Tolterodine tartrate was used as the internal standard (IS). With protein precipitation by acetonitrile and then the simple one-step derivatization, a sensitive bio-assay was achieved with the lower limit of quantitation (LLOQ) as low as 12 ng/mL for plasma. The standard addition calibration curves suitable for clinical sample analysis showed good linearity over the range of 0.012–8.27 mg/mL in plasma and 1.80–84.1 mg/mL in urine. The fully validated method has been successfully applied to a pharmacokinetic study of compound glucosamine sulfate dispersible tablets in health Chinese volunteers receiving single oral doses at 500, 1000 and 1500 mg of glucosamine sulfate, as well as multiple oral doses of 500 mg t.i.d. for 7 consecutive days.展开更多
Simultaneous separation and detection of three organomercury species, namely methylmercury(MeHg),ethylmercury(EtHg), and phenylmercury(PhHg), was performed by using capillary electrophoresis(CE)with UV detection. Pre-...Simultaneous separation and detection of three organomercury species, namely methylmercury(MeHg),ethylmercury(EtHg), and phenylmercury(PhHg), was performed by using capillary electrophoresis(CE)with UV detection. Pre-column derivatization with thiosalicylic acid and on-line salt-induced stacking significantly improved the detection performance. Buffer pH, ion strength, and additive were optimized for CE separation, concentration of NaCl in sample solution and injection time were optimized for on-line stacking. The limits of detection were 76.9,83.0 and 76.4 μg/L for PhHg, EtHg and MeHg, respectively. The developed method was validated by certified reference material and liquid chromatography-atomic fluorescence spectroscopy, which suggests this method could be useful in the speciation of organomercury compounds in biological samples.展开更多
文摘A selective precolumn derivatization liquid chromatography–tandem mass spectrometric (LC–MS/MS) method for the determination of glucosamine in human plasma and urine has been developed and validated. Glucosamine was derivatized by o-phthalaldehyde/3-mercaptopropionic acid. Chromatographic separation was performed on a Phenomenex ODS column (150 mm 4.6 mm, 5 mm) using linear gradient elution by a mobile phase consisting of methanol (A), and an aqueous solution containing 0.2% ammonium acetate and 0.1% formic acid (B) at a flow rate of 1 mL/min. Tolterodine tartrate was used as the internal standard (IS). With protein precipitation by acetonitrile and then the simple one-step derivatization, a sensitive bio-assay was achieved with the lower limit of quantitation (LLOQ) as low as 12 ng/mL for plasma. The standard addition calibration curves suitable for clinical sample analysis showed good linearity over the range of 0.012–8.27 mg/mL in plasma and 1.80–84.1 mg/mL in urine. The fully validated method has been successfully applied to a pharmacokinetic study of compound glucosamine sulfate dispersible tablets in health Chinese volunteers receiving single oral doses at 500, 1000 and 1500 mg of glucosamine sulfate, as well as multiple oral doses of 500 mg t.i.d. for 7 consecutive days.
基金the National Natural Science Foundation of China (No. 21777178)for financial support
文摘Simultaneous separation and detection of three organomercury species, namely methylmercury(MeHg),ethylmercury(EtHg), and phenylmercury(PhHg), was performed by using capillary electrophoresis(CE)with UV detection. Pre-column derivatization with thiosalicylic acid and on-line salt-induced stacking significantly improved the detection performance. Buffer pH, ion strength, and additive were optimized for CE separation, concentration of NaCl in sample solution and injection time were optimized for on-line stacking. The limits of detection were 76.9,83.0 and 76.4 μg/L for PhHg, EtHg and MeHg, respectively. The developed method was validated by certified reference material and liquid chromatography-atomic fluorescence spectroscopy, which suggests this method could be useful in the speciation of organomercury compounds in biological samples.
