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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
Biomedical Chromatography ( IF 1.8 ) Pub Date : 2020-12-07 , DOI: 10.1002/bmc.5042
Zhengcai Ju 1 , Chunyong He 1 , Jia Li 1 , Li Yang 1, 2 , Zhengtao Wang 1, 2
Affiliation  

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 C18 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 NGFt1 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 1.65%–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.

中文翻译:

快速灵敏的超高压液相色谱-串联质谱法测定大鼠血浆中的三七皂苷Ft1及其在药代动力学研究中的应用

三七皂苷Ft1(NGFt1)是从三七中分离出的达玛烷三萜糖苷,在我们先前的测定中显示出有效的刺激血小板聚集的作用,但其药代动力学行为尚不清楚。这项研究描述了一种快速灵敏的超高压液相色谱串联质谱测定法,用于测定大鼠血浆中的NGFt1。甲醇介导的沉淀用于样品预处理。色谱分离是在C 18色谱柱上进行的,使用水和乙腈作为流动相进行梯度洗脱。使用电喷雾电离源以负选择反应监测(SRM)模式在m / z 915.9→  m / z 783.8和m / z的跃迁下进行测定对于NGFt1和内标,分别为799.8→  m / z 637.8。在浓度范围为0.25-2500 ng / mL时线性分析(r  > 0.995),定量下限为0.25 ng / mL。日内和日间精度(相对标准偏差,%)分别为1.65%–9.84%和2.46%–13.49%,而准确性(相对回收率,%)分别为96.21%至99.45%。回收率从95.09%到102.22%,基质效应从98.29%到100.13%。分析物在测试的储存条件下是稳定的。在单次静脉内(2 mg / kg)和口服(50 mg / kg)给药后,该方法已成功应用于大鼠的临床前药代动力学研究。
更新日期:2020-12-07
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