Macek J, Klíma J, Ptácek P
Pharmakl s.r.o., Seydlerova 2451, CZ-15800 Prague 13, Czech Republic.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Jun 1;852(1-2):282-7. doi: 10.1016/j.jchromb.2007.01.026. Epub 2007 Feb 1.
A rapid, sensitive and reliable method was developed to quantitate omeprazole in human plasma using liquid chromatography-tandem mass spectrometry. The assay is based on protein precipitation with acetonitrile and reversed-phase liquid chromatography performed on an octadecylsilica column (55 mm x 2mm, 3 microm particles), the mobile phase consisted of methanol-10 mM ammonium acetate (60:40, v/v). Omeprazole and flunitrazepam, the internal standard, elute at 0.80+/-0.10 min with a total run time 1.35 min. Quantification was through positive ion mode and selected reaction monitoring mode at m/z 346.1-->197.9 for omeprazole and m/z 314.0-->268.0 for flunitrazepam, respectively. The lower limit of quantitation was 1.2 ng/ml using 0.25 ml of plasma and linearity was observed from 1.2 to 1200 ng/ml. Within-day and between-day precision expressed by relative standard deviation was less than 5% and inaccuracy did not exceed 12%. The assay was applied to the analysis of samples from a pharmacokinetic study.
建立了一种快速、灵敏且可靠的方法，采用液相色谱-串联质谱法测定人血浆中的奥美拉唑。该测定法基于用乙腈进行蛋白质沉淀，并在十八烷基硅胶柱（55 mm×2mm，3微米颗粒）上进行反相液相色谱，流动相由甲醇-10 mM醋酸铵（60:40，v/v）组成。奥美拉唑和内标氟硝西泮在0.80±0.10分钟洗脱，总运行时间为1.35分钟。定量通过正离子模式和选择反应监测模式进行，奥美拉唑的质荷比为m/z 346.1→197.9，氟硝西泮的质荷比为m/z 314.0→268.0。使用0.25 ml血浆时定量下限为1.2 ng/ml，在1.2至1200 ng/ml范围内观察到线性关系。日内和日间精密度以相对标准偏差表示小于5%，误差不超过12%。该测定法应用于药代动力学研究样品的分析。
