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建立一种简便、高灵敏度的液相串联质谱分析方法测定人血浆中妥洛特罗的浓度。以异丙醇–正己烷(5:95,v/v)为提取试剂,妥洛特罗-d9为内标,使用300 Extend C_(18)(4.6 mm×150 mm,5μm)为分析柱对妥洛特罗进行分离。流动相为0.1%甲酸水(A)–乙腈(B),等梯度洗脱,流速为1.0 mL/min,1:1进行分流。采用多反应监测模式,正离子扫描对妥洛特罗进行定量分析,妥洛特罗及内标的定量离子对分别为m/z 228.1→m/z 154.0和m/z 237.2→m/z 154.0.血浆中妥洛特罗线性范围为0.01–5.0 ng/mL,定量下限为0.01 ng/mL。日间精密度<3.7%,日内精密度<11.1%。绝对回收率高于66%,基质效应影响较小。该方法可应用于健康受试者使用妥洛特罗透皮贴剂后的药代动力学研究。
A simple and sensitive liquid chromatography-tandem mass spectrometry method was established for the determination of tulobuterol in human plasma. The extraction was performed with isopropanol-n-hexane (5:95, v / v) and tulobuterol-d9 was used as the internal standard and 300 Extend C 18 (4.6 mm × 150 mm, 5μm) Tulobuterol for separation. The mobile phase consisted of 0.1% formic acid in water (A) -acetonitrile (B) with equal gradient elution at a flow rate of 1.0 mL / min and a 1: 1 split. Quantitative analysis of tulobron was performed by multi-reaction monitoring and positive ion scanning. The quantitative ion pairs of tulobuterol and internal standard were m / z 228.1 → m / z 154.0 and m / z 237.2 → m / z 154.0, respectively. The linear range of tulobuterol in plasma ranged from 0.01 to 5.0 ng / mL with a lower limit of quantitation of 0.01 ng / mL. Daytime precision <3.7%, day precision <11.1%. The absolute recovery is higher than 66%, with less effect of matrix effect. The method is applicable to pharmacokinetic studies of tulobuterol transdermal patches in healthy subjects.