液质联用（LC-MS）法检测特拉唑嗪及应用

目的：建立液质联用（LC-MS）法测定人体血浆特拉唑嗪的浓度及应用。方法：岛津LC-MS2010液相色谱-质谱联用仪,色谱柱为Thermo Hypersil-Hypurity C18（150mm×2.1mm,5μm）;柱温：40℃;流动相为20mmmol/L乙酸铵溶液（pH4.3）∶甲醇∶乙腈=65∶20∶15;流速：0.25mL/min。采用电喷雾正离子模式离子化,用于定量分析的离子分别为m/z388（特拉唑嗪）、m/z384（哌唑嗪）。血浆样品采用3mol/L氢氧化钠碱化、二氯甲烷萃取后LC-MS测定。进样体积为5μL,样品室温度为5℃。结果：特拉唑嗪线性范围为0.25～50ng/mL,最小定量浓度为0.25ng/mL,提取回收率均〉70%,方法回收率为96.0%～97.6%,日间、日内RSD均〈15%。方法灵敏、稳定、特异性高,并已成功地应用到人体血浆特拉唑嗪药代动力学的研究。结论：该方法简便、准确、重复性好,可以准确地定量人体血浆特拉唑嗪的浓度,适于特拉唑嗪生物利用度和生物等效性的研究。

LC-MS determination of terazosin in human plasma and application

AIM：To develop an LC-MS method to determin the concentration of terazosin in human plasma and its application. METHODS：Shimadzu 2010 LC-MS and Thermo Hypersil-Hypurity C18（150 mm×2.1 mm,5 μm） were used in the experiment. The column temperature was set at 40 ℃. 20 mmol/L ammonium acetate-methanol-acetonitrile（65：20：15,V/V/V） was used as mobile phase and the flow rate was 0.25 mL/min. Ion mass spectral（m/z） of 388,384 were selected to quantify terazosin,prazosin （internal standard）,respectively. The plasma sample were alkalinized with 3 mol/L sodium hydroxide buffer and extracted with dichloromethane. The sample room temperature was set at 5 ℃ and the injection volume was 5 μL. RESULTS：Terazosin was linear range from 0.25-50 ng/mL respectively,the limitation of terazosin was about 0.25 ng/mL. The extraction recoveries from plasma was more than 70%,method recovery was 96.0%-97.6%,the intraday and interday precisions were less than 15%. The method was high sensitivity,stability and specificity and has already been used for pharmacokinetics study of terazosin in human successfully. CONCLUSION：The method is simple,accurate,repetitive for the determination of terazosin in human plasma and suitable for bioavailability and bioequivalence study of terazosin.