Li Zhan, Yao Jing, Zhang Ziqiang, Zhang Luyong
Nanjing Changao Pharmaceutical Science and Technology Limited Company, Nanjing 210022, China.
J Chromatogr Sci. 2009 Nov-Dec;47(10):881-4. doi: 10.1093/chromsci/47.10.881.
A liquid chromatography coupled with mass spectrometry method was developed and validated to determine omeprazole and domperidone simultaneously in dog plasma. Chromatographic separation was performed on a Narrow Bore C(18) column using methanol-10 mM ammonium acetate (68:32, v/v) as the mobile phase at the flow rate of 0.2 mL/min. The chromatographic separation was achieved in less than 7 min. Diazepam was used as the internal standard. Quantitative analysis was achieved by mass spectrometry detection using a mass spectrometer equipped with an electrospray ionization interface and operated in selected ion monitoring and positive ion mode using target ions at m/z 346 for omeprazole, m/z 426 for domperidone, and m/z 285 for internal standard, respectively. The lower limit of quantification was 1 ng/mL and a linear range of 1-200 ng/mL. The intra- and inter-day relative standard deviation was both less than 10%, and the accuracy values were higher than 90%. The method is sensitive and repeatable enough to be used in pharmacokinetic and bioavailability studies.
建立并验证了一种液相色谱-质谱联用方法，用于同时测定犬血浆中的奥美拉唑和多潘立酮。采用窄径C(18)柱进行色谱分离，以甲醇-10 mM醋酸铵(68:32, v/v)为流动相，流速为0.2 mL/min。在不到7分钟内实现了色谱分离。地西泮用作内标。通过配备电喷雾电离接口的质谱仪进行质谱检测，在选择离子监测和正离子模式下操作，分别使用m/z 346的目标离子测定奥美拉唑、m/z 426的目标离子测定多潘立酮、m/z 285的目标离子测定内标，从而实现定量分析。定量下限为1 ng/mL，线性范围为1-200 ng/mL。日内和日间相对标准偏差均小于10%，准确度值高于90%。该方法灵敏度和重复性足以用于药代动力学和生物利用度研究。
