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Abstract：
A simple, fast and sensitive LC-MS/MS method was developed to quantify terazosin in human plasma. The mobile phase consisted of acetonitrile-0.1% (v/v) formic acid (70:30, v/v). Prazosin was used as internal standard (IS). As deproteinization agent, acetonitrile produced a clean sample. A higher response intensity with more symmetrical peak was obtained using Agilent Poroshell 120 EC-C18 - Fast LC column (100 × 2.1mmID, 2.7 μm) compared with Kinetex XB-C18 (100 × 2.1 mm, 2.6 µm) column. The response of terazosin and IS were approximately two times in citrate phosphate dextrose (CPD) plasma compared with dipotassium ethylenediaminetetraacetic acid (K2EDTA) plasma. Plasma calibration curve was linear from 1.0 to 100.0 ng/mL, with coefficient of determination r2 ≥ 0.99. The within-run and between-run precision values (CV, %) were <5.2% and <7.8%, while accuracy values were 102.8-112.7% and 103.4-112.2%. The extended run accuracy was 98.6-102.8% and precision (CV, %) 4.3-10.4%. The recovery of analyte was >98% and IS >94%. Terazosin in plasma kept at benchtop was stable for 24 h, in autosampler tray for 48 h, in instrumentation room for 48 h, for 7 freeze-thaw cycles and in freezer for 140 days. Terazosin and IS stock standard solutions were stable for 140 days at room temperature and in the chiller. The high throughput method was successfully utilized to measure 935 samples in a bioequivalence study of terazosin.
摘要：
一个简单的，建立了快速灵敏的LC-MS/MS方法来定量人血浆中的特拉唑嗪。流动相由乙腈-0.1%(v/v)甲酸(70:30,v/v)组成。哌唑嗪用作内标(IS)。作为脱蛋白剂，乙腈产生干净的样品。使用AgilentPoroshell120EC-C18-FastLC色谱柱（100×2.1mmID，2.7μm)与KinetexXB-C18(100×2.1mm,2.6µm)柱。与乙二胺四乙酸二钾（K2EDTA）血浆相比，柠檬酸盐磷酸葡萄糖（CPD）血浆中特拉唑嗪和IS的反应约为2倍。血浆校准曲线在1.0至100.0ng/mL范围内呈线性关系，决定系数r2≥0.99。运行内和运行间精度值(CV,%)分别为<5.2%和<7.8%，而准确度值分别为102.8-112.7%和103.4-112.2%。扩展运行精度为98.6-102.8%，精度为(CV，%）4.3-10.4%。分析物的回收率>98%,IS>94%。特拉唑嗪在血浆中保持在台式稳定24小时，在自动进样器托盘中48小时，在仪表室48小时，进行7次冻融循环，并在冰箱中放置140天。特拉唑嗪和IS储备标准溶液在室温和冷却器中稳定140天。在特拉唑嗪的生物等效性研究中，高通量方法已成功用于测量935个样品。
