van Rooyen G F, Smit M J, De Jager A D, Hundt H K L, Swart K J, Hundt A F
FARMOVS-PAREXEL, Clinical Research Organisation, Brandhof, South Africa.
J Chromatogr B Analyt Technol Biomed Life Sci. 2002 Mar 5;768(2):223-9. doi: 10.1016/s1570-0232(01)00566-9.
A sensitive method for the determination of clarithromycin in plasma is described, using high-performance liquid chromatographic separation with tandem mass spectrometric detection. Samples were prepared using liquid-liquid extraction and separated on a Supelco Discovery C18 column with a mobile phase consisting of acetonitrile, methanol and acetic acid. Detection was performed by a PE SCIEX API 2000 mass spectrometer in the multiple reaction monitoring (MRM) mode (LC-MS-MS) using TurbolonSpray ionization and monitoring the transition of the protonated molecular ion for clarithromycin at m/z 748.5 (M+1) to the predominant product ion of m/z 158.2. The mean recovery of clarithromycin was 87.3%, with a lower limit of quantification of 2.95 ng/ml when using 0.3-ml plasma. This high-throughput method was used to quantify 230 samples per day, and is sufficiently sensitive to be employed in pharmacokinetic studies.
本文描述了一种测定血浆中克拉霉素的灵敏方法，该方法采用高效液相色谱分离与串联质谱检测。样品采用液液萃取法制备，并在Supelco Discovery C18柱上进行分离，流动相由乙腈、甲醇和乙酸组成。检测采用PE SCIEX API 2000质谱仪，在多反应监测（MRM）模式（LC-MS-MS）下，使用TurbolonSpray离子化方式，监测克拉霉素质子化分子离子m/z 748.5（M+1）到主要产物离子m/z 158.2的跃迁。当使用0.3 ml血浆时，克拉霉素的平均回收率为87.3%，定量下限为2.95 ng/ml。这种高通量方法每天可定量230个样品，灵敏度足以用于药代动力学研究。
