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目的:建立测定人血浆中卡维地洛浓度的LC/MS方法。方法:以盐酸氨溴索为内标,待测血浆样品经乙腈沉淀,高速离心后取上清液进样,色谱柱为SHIMADZU VP-ODS柱(250 mm×2.0 mm,5μm),甲醇-0.1%甲酸水溶液=64:36(含10 mmol·L~(-1)乙酸铵)为流动相。ESI离子源;CDL Tempe 250℃,Heat Block Tempe 200℃,Detector Voltage 1.7 Kv;正离子方式检测,扫描方式为选择离子扫描(SIM),用于定量的离子分别为卡维地洛m/z:407;内标(氨溴索)m/z:379;扫描时间:0.2 s。结果:内源性物质不干扰卡维地洛的检测,每个样品分析时间约4.4 min,卡维地洛的线性范围为0.3～120 ng·ml~(-1),批内、批间RSD均小于10%,低、中、高浓度的(0.6,5,60 ng·ml~(-1))平均提取回收率分别为92.43%、85.08%、88.32%。结论:该法操作快速、简单、准确,介质用量少,可用于临床药物动力学研究中大批量血样的处理。
Objective: To establish a LC / MS method for the determination of carvedilol in human plasma. Methods: Ambroxol hydrochloride was used as internal standard. Plasma samples were precipitated with acetonitrile. After centrifugation, the supernatant was injected into the sample. The column was SHIMADZU VP-ODS column (250 mm × 2.0 mm, 5 μm) % Aqueous solution of formic acid = 64:36 (containing 10 mmol·L -1 ammonium acetate) as the mobile phase. ESI ion source; CDL Tempe 250 ℃, Heat Block Tempe 200 ℃, Detector Voltage 1.7 Kv; positive ion mode detection, scanning mode is selected ion scan (SIM), the ions used for quantification are carvedilol m / z: 407; internal standard (ambroxol) m / z: 379; scan time: 0.2 s. Results: The endogenous substances did not interfere with the detection of carvedilol. The analysis time of each sample was about 4.4 min. The linear range of carvedilol was 0.3 ~ 120 ng · ml ~ (-1). Intra- and inter-assay RSD The average recoveries of low, medium and high concentrations (0.6, 5, 60 ng · ml -1) were 92.43%, 85.08% and 88.32%, respectively. Conclusion: The method is fast, simple and accurate, with less dosage. It can be used in the treatment of high-volume blood samples in clinical pharmacokinetic studies.