采用液相色谱-串联质谱法定量测定人血浆中的补骨脂呋喃。
Quantitative determination of buagafuran in human plasma by liquid chromatography-tandem mass spectrometry.
机构信息
Clinical Pharmacology Research Center, Peking Union Medical College Hospital and Chinese Academy of Medical Sciences, Beijing 100730, China.
出版信息
J Chromatogr B Analyt Technol Biomed Life Sci. 2011 Jun 15;879(20):1789-94. doi: 10.1016/j.jchromb.2011.04.029. Epub 2011 May 6.
A sensitive and selective high performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed for the determination of buagafuran in human plasma. The analyte was extracted from plasma samples with hexane after addition of isotopic internal standard and chromatographed on a RP-C(8) column. The mobile phase consisted of methanol-water (90:10, v/v) and the flow rate was 0.2 mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reactions monitoring (MRM) mode using positive electrospray ionization (ESI). The method was validated over the concentration range of 0.5-200 ng/mL. Inter- and intra-day precision (RSD%) were all within 15% and the accuracy (RE%) was equal or lower than 9.5%. The lower limit of quantitation (LLOQ) was 0.5 ng/mL. The extraction recovery was on average 38.1% and the detection was not affected by the matrix. The method was successfully applied to the pharmacokinetic study of buagafuran in healthy Chinese volunteers.
建立了一种灵敏、选择性的高效液相色谱-串联质谱（HPLC-MS/MS）法，用于测定人血浆中的补骨脂呋喃。分析物在加入同位素内标后，用正己烷从血浆样品中提取，在 RP-C（8）柱上进行色谱分离。流动相由甲醇-水（90:10，v/v）组成，流速为 0.2 mL/min。检测采用三重四极杆串联质谱，在多重反应监测（MRM）模式下进行，采用正电喷雾电离（ESI）。该方法在 0.5-200 ng/mL 的浓度范围内进行了验证。日内和日间精密度（RSD%）均在 15%以内，准确度（RE%）等于或低于 9.5%。定量下限（LLOQ）为 0.5 ng/mL。平均提取回收率为 38.1%，且检测不受基质影响。该方法成功应用于健康中国志愿者中补骨脂呋喃的药代动力学研究。
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