Smit M J, Sutherland F C W, Hundt H K L, Swart K J, Hundt A F, Els J
Farmovs-Parexel Clinical Research Organisation, Bioanalytical Sciences Division, Brandhof, South Africa.
J Chromatogr A. 2002 Mar 8;949(1-2):65-70. doi: 10.1016/s0021-9673(01)01553-9.
A rapid and sensitive method for the determination of domperidone in plasma was developed, using high-performance liquid chromatographic separation with tandem mass spectrometry detection. The samples were rendered basic with 1 M Na2CO3 and the domperidone extracted using tert.-butyl methyl ether, followed by back-extraction into formic acid (2% in water). Chromatography was performed on a Phenomenex Luna C8 (2), 5 microm, 150x2 mm column with a mobile phase consisting of acetonitrile-0.02% formic acid (300:700, v/v), delivered at 0.2 ml/min. Detection was performed using an Applied Biosystems Sciex API 2000 mass spectrometer set at unit resolution in the multiple reaction monitoring mode. TurbolonSpray ionisation was used for ion production. The mean recovery of domperidone was +/- 100%, with a lower limit of quantification set at 0.189 ng/ml. This assay method makes use of the increased sensitivity and selectivity of tandem mass spectrometric detection resulting in a rapid (extraction and chromatography) and sensitive method for the determination of domperidone in human plasma, which is more sensitive than previously described methods.
建立了一种快速灵敏的血浆中多潘立酮测定方法，采用高效液相色谱分离-串联质谱检测。样品用1 M碳酸钠碱化，多潘立酮用叔丁基甲醚萃取，然后反萃取到甲酸（2%水溶液）中。在Phenomenex Luna C8（2）、5μm、150×2 mm柱上进行色谱分析，流动相为乙腈-0.02%甲酸（300:700，v/v），流速为0.2 ml/min。使用Applied Biosystems Sciex API 2000质谱仪在多反应监测模式下以单位分辨率进行检测。采用TurbolonSpray离子化进行离子产生。多潘立酮的平均回收率为±100%，定量下限设定为0.189 ng/ml。该测定方法利用了串联质谱检测提高的灵敏度和选择性，从而形成了一种快速（萃取和色谱）且灵敏的人血浆中多潘立酮测定方法，比先前描述的方法更灵敏。
