Niu Zhanqi, Chen Fengju, Sun Jin, Liu Xiaohong, Wang Yongjun, Chen Dawei, He Zhonggui
Department of Biopharmaceutics, School of Pharmacy, Shenyang Pharmaceutical University, No. 103, Wenhua Road, Shenyang 110016, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2008 Jul 1;870(1):135-9. doi: 10.1016/j.jchromb.2008.05.044. Epub 2008 Jun 4.
A rapid, sensitive and specific high performance liquid chromatography-electrospray ionization tandem quadrupole mass spectrometry (HPLC-MS/MS) method was developed and validated for the determination of 3-n-butylphthalide in rat plasma. Following protein precipitation with acetonitrile, 3-n-butylphthalide and glipizide (internal standard, I.S.) were separated using a gradient elution program on a C18 column and detected by mass spectrometry in positive ion mode with the multiple reaction monitoring (MRM) mode using the respective precursor to product ion combinations of m/z 191/145 for 3-n-butylphthalide and m/z 446/321 for glipizide, respectively. The total chromatographic running time was 2.5 min. The method was linear over the concentration range of 11.14-3480.00 ng/mL, using as little as 100 microL plasma. The lower limit of quantification (LLOQ) was 5.57 ng/mL. Finally, the method was successfully used to support a preclinical pharmacokinetic study of 3-n-butylphthalide in rats following intravenous administration.
建立了一种快速、灵敏且特异的高效液相色谱-电喷雾电离串联四极杆质谱法（HPLC-MS/MS），并对其进行了验证，用于测定大鼠血浆中的3-正丁基苯酞。用乙腈进行蛋白沉淀后，3-正丁基苯酞和格列吡嗪（内标，I.S.）在C18柱上采用梯度洗脱程序进行分离，并通过质谱在正离子模式下以多反应监测（MRM）模式进行检测，3-正丁基苯酞的质荷比为m/z 191/145，格列吡嗪的质荷比为m/z 446/321。总色谱运行时间为2.5分钟。该方法在11.14 - 3480.00 ng/mL的浓度范围内呈线性，血浆用量低至100微升。定量下限（LLOQ）为5.57 ng/mL。最后，该方法成功用于支持大鼠静脉注射3-正丁基苯酞后的临床前药代动力学研究。
