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首页> 外文期刊>Biomedical Chromatography: An International Journal Devoted to Research in Chromatographic Methodologies and Their Applications in the Biosciences >A rapid and sensitive ultra-high-pressure liquid chromatography-tandem mass spectrometry method for the determination of notoginsenoside Ft1 in rat plasma with application to pharmacokinetic study
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A rapid and sensitive ultra-high-pressure liquid chromatography-tandem mass spectrometry method for the determination of notoginsenoside Ft1 in rat plasma with application to pharmacokinetic study

机译:一种快速敏感的超高压液相色谱 - 串联质谱法测定大鼠等离子体中的非血糖钠FT1,应用于药代动力学研究

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摘要

Notoginsenoside Ft1 (NGFt1), a dammarane triterpene glycoside isolated from Panax notoginseng, showed potent effective in stimulating platelet aggregation in our previous assay, yet its pharmacokinetic behavior is still unclear. This study describes a rapid and sensitive ultra-high-pressure LC-tandem mass spectrometry assay for determining of NGFt1 in rat plasma. Methanol-mediated precipitation was used for sample pre-treatment. Chromatographic separation was achieved on a C_18 column with gradient elution using water and acetonitrile as mobile phase. Determination was obtained using an electrospray ionization source in negative selected reaction monitoring (SRM) mode at the transitions of m/z 915.9 → m/z 783.8 and m/z 799.8 →m/z 637.8 for NGFtl and internal standard, respectively. The assay was linear over the concentration range 0.25-2500 ng/mL (r > 0.995) with the lower limit of quantification of 0.25 ng/mL The intra- and inter-day precisions (relative standard deviation, %) ranged 1.6556-9.84% and 2.46%-13.49%, respectively, whereas accuracy (relative recovery, %) ranged from 96.21% to 99.45%, respectively. The recovery ranged from 95.09% to 102.22% and the matrix effect from 98.29% to 100.13%. The analyte was stable under tested storage conditions. The method has been successfully applied to a preclinical pharmacokinetic study in rats after a single intravenous (2 mg/kg) and oral (50 mg/kg) administration.
机译:Notoginsenaine FT1(NGFT1)是从Panax Notoginseg中分离的达莫烷苷糖苷,在我们之前的测定中刺激血小板聚集的有效有效,但其药代动力学行为尚不清楚。该研究描述了一种快速敏感的超高压LC串联质谱法测定,用于确定大鼠等离子体中的NgFT1。甲醇介导的沉淀用于样品预处理。在C_18塔上实现色谱分离,使用水和乙腈作为流动相的梯度洗脱。在NGFT1和NgFT1和内标的M / Z 915.9→M / Z 783.8和M / Z 637.8的过渡处,在负选中反应监测(SRM)模式下的电喷雾电离源获得测定。测定在0.25-2500ng / ml(r> 0.995)的浓度范围内线性,其定量下限为0.25ng / ml,血液和日间诊断(相对标准偏差,%)范围为1.6556-9.84%分别为2.46%-13.49%,而准确性(相对恢复,%)分别为96.21%至99.45%。恢复从95.09%到102.22%,基质效应为98.29%至100.13%。分析物在测试的储存条件下稳定。该方法已成功应用于单个静脉内(2mg / kg)和口服(50mg / kg)给药后大鼠的临床前药代动力学研究。

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