Van Rooyen G F, Badenhorst D, Swart K J, Hundt H K L, Scanes T, Hundt A F
FARMOVS-PAREXEL Clinical Research Organisation, Brandhof, South Africa.
J Chromatogr B Analyt Technol Biomed Life Sci. 2002 Mar 25;769(1):1-7. doi: 10.1016/s1570-0232(01)00590-6.
A sensitive method for the determination of carbamazepine and carbamazepine 10,11-epoxide in plasma is described, using high-performance liquid chromatographic separation with tandem mass spectrometry. Samples were purified using liquid-liquid extraction and separated on a Phenomenex Luna C18 5 microm. 150 x 2 mm column with a mobile phase consisting of acetonitrile, methanol and formic acid (0.1%) (10:70:20, v/v). Detection was performed by a Micromass Quattro Ultima mass spectrometer in the MRM mode (LC-MS-MS) using electro spray ionisation (ESI+), monitoring the transition of the protonated molecular ion for carbamazepine at m/z 237.05 and carbamazepine 10,11-epoxide at m/z 253.09 to the predominant ions of m/z 194.09 and 180.04, respectively. The mean recovery was 95% for carbamazepine and 101% for carbamazepine 10,11-epoxide, with a lower limit of quantification of 0.722 ng/ml for carbamazepine and 5.15 ng/ml for carbamazepine 10,11-epoxide, when using 0.5 ml plasma. This high-throughput method was used to quantify 230 samples per day, and is sufficiently sensitive to be employed in pharmacokinetic studies.
本文描述了一种采用高效液相色谱-串联质谱法测定血浆中卡马西平和卡马西平10,11-环氧化物的灵敏方法。样品经液-液萃取纯化后，在Phenomenex Luna C18 5微米、150×2毫米的色谱柱上进行分离，流动相由乙腈、甲醇和0.1%甲酸（10:70:20，v/v）组成。采用Micromass Quattro Ultima质谱仪在MRM模式（LC-MS-MS）下，通过电喷雾电离（ESI+）进行检测，监测卡马西平质子化分子离子m/z 237.05和卡马西平10,11-环氧化物质子化分子离子m/z 253.09分别到主要离子m/z 194.09和180.04的跃迁。当使用0.5毫升血浆时，卡马西平的平均回收率为95%，卡马西平10,11-环氧化物的平均回收率为101%，卡马西平的定量下限为0.722纳克/毫升，卡马西平10,11-环氧化物的定量下限为5.15纳克/毫升。这种高通量方法每天可定量分析230个样品，灵敏度足以用于药代动力学研究。
