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目的:建立液相色谱串联质谱法测定人血浆中伪人参皂苷GQ浓度。方法:血浆样品中加入适量内标,以乙酸乙酯萃取后采用Waters Xevo TQS LC-MS/MS进行分析。采用Poroshell 120 EC C8色谱柱(2.1 mm×50 mm,2.7μm),柱温40℃,以甲醇-10 mmol·L-1醋酸铵水溶液(80∶20)为流动相,流速0.3 m L·min-1;采用多反应离子监测(MRM)的扫描模式,以电喷雾离子源(ESI)在负离子电离模式下进行测定。结果:本方法的线性范围为2.500~5 000 ng·m L-1,最低定量限为2.500 ng·m L-1,日内、日间精密度均小于15%,准确度在85%~115%之间,萃取回收率约9%~11%,基质效应约66%~73%,稳定性考察结果良好。药动学试验结果表明,静注伪人参皂苷GQ 120 mg·次-1,每日1次,连续用药5 d后,达峰时间为2 h,半衰期约10 h。试验第1 d和第5 d主要药代动力学参数基本一致,计算蓄积系数分别是RC max=0.964±0.099,和RAUC=0.965±0.181,两者均接近1。结论:本方法适用于伪人参皂苷GQ的人体药代动力学研究。在本文给药方案下,伪人参皂苷GQ在人体内没有明显蓄积现象,连续给药不影响伪人参皂苷GQ的人体药代动力学过程。
Objective: To establish a method for the determination of ginsenoside GQ in human plasma by liquid chromatography-tandem mass spectrometry. Methods: An appropriate amount of internal standard was added to the plasma samples and extracted with ethyl acetate. The samples were analyzed by Waters Xevo TQS LC-MS / MS. A Poroshell 120 EC C8 column (2.1 mm × 50 mm, 2.7 μm) was used with a mobile phase of methanol-10 mmol·L-1 ammonium acetate (80:20) at a flow rate of 0.3 m L · min -1; Scanning mode using multiple reaction ion monitoring (MRM) with electrospray ionization source (ESI) in negative ionization mode. Results: The linear range of this method was 2.500 ~ 5 000 ng · m L-1, the minimum limit of quantification was 2.500 ng · m L-1. The precision of the method was less than 15%, with the accuracy of 85% -115% Between the recovery of about 9% to 11%, the matrix effect of about 66% to 73%, the stability of the study results were good. Pharmacokinetic test results showed that intravenous injection of pseudo-ginsenoside GQ 120 mg · times -1 once a day for 5 days after continuous administration, the peak time of 2 h, half-life of about 10 h. The main pharmacokinetic parameters on day 1 and day 5 of the trial were basically the same. The calculated accumulation coefficients were RC max = 0.964 ± 0.099 and RAUC = 0.965 ± 0.181, both of which were close to 1. Conclusion: This method is suitable for the study of human pharmacokinetics of pseudoginsenoside GQ. Under this dosing regimen, pseudo-ginsenoside GQ has no obvious accumulation in human body, and continuous administration does not affect human pharmacokinetics of pseudo-ginsenoside GQ.