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目前多沙唑嗪及其对映体的生物样本最低定量限未超过0.1 ng·m L~(-1),本研究建立了一种新的大鼠血浆左旋多沙唑嗪微量检测液相色谱-串联质谱(LC-MS/MS)方法。血浆样本加入内标哌唑嗪后经C18固相萃取小柱萃取,碱性条件下采用Acquity BEH C_(18)(50 mm×2.1 mm,1.7μm)色谱柱进行分离,在正离子模式下以MRM(多反应离子监测)方式测定左旋多沙唑嗪的含量。结果表明,左旋多沙唑嗪在10.4 pg·m L~(-1)~13 ng·m L~(-1)范围内线性关系良好(r=0.992 2),最低定量限为10.4 pg·m L~(-1)。采用提取后加入法及柱后灌注法评价血浆样本的基质效应,不存在明显的基质效应。并用本法可测定大鼠尾静脉注射左旋多沙唑嗪(3 mg·kg-1)48 h后的血药浓度,结果为0.034 4±0.010 2 ng·m L~(-1)。此方法特异性强,灵敏度高,适用于左旋多沙唑嗪的血药浓度测定,也为其他药物血药浓度的分析提供了参考。
At present, the lowest limit of quantification of doxazosin and its enantiomers does not exceed 0.1 ng · m L -1. In this study, we developed a new method for the determination of levodopa in rat plasma - Tandem mass spectrometry (LC-MS / MS) method. The plasma samples were extracted with internal standard prazosin and extracted with C18 solid phase extraction column. The samples were separated on a Acquity BEH C 18 (50 mm × 2.1 mm, 1.7 μm) column under alkaline conditions. In the positive ion mode MRM (multi-reactive ion monitoring) method for the determination of levodopazazine content. The results showed that there was a good linear relationship (r = 0.992 2) in the range of 10.4 pg · m L -1 to 13 ng · m L -1 with the lowest limit of quantification being 10.4 pg · m L ~ (-1). The matrix effects of plasma samples were evaluated using post-injection and post-column perfusion methods without significant matrix effects. The plasma concentration of levodopa zoxadiazine (3 mg · kg -1) administered to the tail vein of rats after 48 h was determined by this method. The result was 0.034 4 ± 0.010 2 ng · m L -1. This method is of high specificity and high sensitivity, suitable for the determination of levodopa zoxal in plasma concentration, but also provide a reference for the analysis of other drugs blood concentration.