School of Pharmacy, Hebei Medical University, 361 East Zhongshan Road, 050017 Shijiazhuang, China.
J Pharm Biomed Anal. 2011 Dec 15;56(5):1101-5. doi: 10.1016/j.jpba.2011.07.043. Epub 2011 Aug 16.
A novel and sensitive method utilizing high performance liquid chromatography coupled with electrospray ionization source tandem mass spectrometry (LC-ESI-MS(3)) was developed for the first time in order to analyze nitrendipine in human plasma samples. Human plasma samples were prepared by protein precipitation with acetonitrile and well resolved on a 100 mm reversed-phase column in gradient elution with 0.05% (v/v) formic acid in acetonitrile as the mobile phase. Determination was performed in MS(3) scan mode for nitrendipine and in the multiple reaction monitoring (MRM) mode for nimodipine (internal standard). This method, having a lower limit of quantification (LLOQ) of 0.05 ng/mL when using a 100 μL sample aliquot (5 pg/sample), is acceptable for calibration of the linearity and repeatability and is of better sensitivity than the reported methods (>0.25 ng/mL). The major advantages of the method are that small sample volume (100 μL) is required, simple sample processing technique, high sensitivity and excellent selectivity is guaranteed by the MS(3) detection. The proposed validated method has been successfully applied to a clinical study on nitrendipine.
首次建立了利用高效液相色谱-电喷雾串联质谱（LC-ESI-MS(3)）检测人血浆样品中尼群地平的新方法。采用乙腈沉淀蛋白法处理人血浆样品，在 100mm 反相柱上以 0.05%（v/v）甲酸乙腈为流动相进行梯度洗脱，实现了尼群地平的良好分离。采用 MS(3)扫描模式对尼群地平进行定量分析，采用内标法（尼莫地平）进行多重反应监测（MRM）模式检测。该方法在使用 100μL 样品（5pg/sample）时，定量下限（LLOQ）为 0.05ng/mL，可接受线性和重复性校准，且灵敏度优于报道方法（>0.25ng/mL）。该方法的主要优点是所需样品体积小（100μL），样品处理技术简单，MS(3)检测保证了高灵敏度和出色的选择性。所建立的方法已成功应用于尼群地平的临床研究。
