超高效液相色谱-串联质谱法对大鼠血浆中一种新型抗菌肽的定量分析
Quantitative analysis of a novel antimicrobial peptide in rat plasma by ultra performance liquid chromatography-tandem mass spectrometry.
作者信息
Zhang Ruo-Wen, Liu Wen-Tao, Geng Lu-Lu, Chen Xiao-Hui, Bi Kai-Shun
机构信息
School of Pharmacy, Shenyang Pharmaceutical University, Shenyang 110016, China.
School of Pharmacy, Medical Biology Centre, Queen's University Belfast, UK.
出版信息
J Pharm Anal. 2011 Aug;1(3):191-196. doi: 10.1016/j.jpha.2011.04.001. Epub 2011 Jul 26.
We described the first results of a quantitative ultra performance liquid chromatography-tandem mass spectrometry method for a novel antimicrobial peptide (phylloseptin, PSN-1). Chromatographic separation was accomplished on a Waters bridged ethyl hybrid (BEH) C (50 mm×2.1 mm, 1.7 μm) column with acetonitrile-water (25:75, v/v) as isocratic mobile phase. Mass spectrometry detection was performed in the positive electrospray ionization mode and by monitoring of the transitions at / 679.6/120, 509.6/120 (PSN-1) and /z 340.7/165 (Thymopentin, IS). Protein precipitation was investigated and the recovery was satisfactory (above 82%). The method was shown to be reproducible and reliable with intra-day precision below 5.3%, inter-day precision below 14.2%, and linear range from 0.02 to 2 μg/mL with >0.994. The method was successfully applied to a pharmacokinetic study of PSN-1 in rats after intravenous administration.
我们描述了一种用于新型抗菌肽（叶形抗菌肽，PSN-1）的定量超高效液相色谱-串联质谱法的初步结果。色谱分离在沃特世桥接乙基杂化（BEH）C18柱（50 mm×2.1 mm，1.7μm）上进行，以乙腈-水（25:75，v/v）作为等度流动相。质谱检测在正电喷雾电离模式下进行，通过监测m/z 679.6/120、509.6/120（PSN-1）和m/z 340.7/165（胸腺五肽，内标）的跃迁。对蛋白沉淀进行了研究，回收率令人满意（高于82%）。该方法具有重现性和可靠性，日内精密度低于5.3%，日间精密度低于14.2%，线性范围为0.02至2μg/mL，相关系数>0.994。该方法已成功应用于大鼠静脉注射PSN-1后的药代动力学研究。
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