Paglia G, D'Apolito O, Garofalo D, Scarano C, Corso G
Clinical Biochemistry, Department of Biomedical Sciences, University of Foggia, Foggia, Italy.
J Chromatogr B Analyt Technol Biomed Life Sci. 2007 Dec 15;860(2):153-9. doi: 10.1016/j.jchromb.2007.10.025. Epub 2007 Oct 25.
A fast, sensitive and specific LC/MS/MS method for the simultaneous analysis of oxcarbazepine (OXC), 10-hydroxycarbazepine (MHD) and trans-diol-carbazepine (DHD), in human serum, has been developed and validated. Serum drugs were extracted by C8 solid-phase cartridges (SPE) and separated in less than 3 min on a C18 reverse-phase column using an isocratic elution. A tandem mass spectrometer, as detector, was used for quantitative analysis in positive mode by a multiple reaction monitoring. Calibration curves, obtained on two ranges of concentration (0.78-50 mg/L for MHD and 0.078-5.0 mg/L for OXC and DHD), showed correlation coefficients (r) better than 0.997. Within day and between days quality controls imprecision, as CV%, ranged from 0.3 to 4.6% and from 1.9 to 5.8%, respectively. Cyheptamide (CYE) was used as internal standard. No detectable carry-over and no relevant cross-talk and matrix effect occurred. Samples from 24 treated patients were analysed and drug serum concentrations obtained by this method are in agreement with those of other methods and also are well correlated (r=0.88) in comparison to our routine HPLC-UV method. Based on the analytical results and short run time, the method is suitable to support routine analysis of therapeutic drugs monitoring from human serum of treated patients or for pharmacokinetic studies.
已开发并验证了一种快速、灵敏且特异的液相色谱/串联质谱法，用于同时分析人血清中的奥卡西平（OXC）、10-羟基卡马西平（MHD）和反式二醇卡马西平（DHD）。血清药物通过C8固相萃取柱（SPE）提取，并在C18反相柱上使用等度洗脱在不到3分钟内分离。使用串联质谱仪作为检测器，通过多反应监测在正模式下进行定量分析。在两个浓度范围内（MHD为0.78 - 50 mg/L，OXC和DHD为0.078 - 5.0 mg/L）获得的校准曲线显示相关系数（r）优于0.997。日内和日间质量控制的不精密度，以CV%计，分别为0.3%至4.6%和1.9%至5.8%。赛庚酰胺（CYE）用作内标。未检测到残留，也未出现相关的串扰和基质效应。分析了24例接受治疗患者的样本，该方法获得的药物血清浓度与其他方法一致，并且与我们的常规高效液相色谱 - 紫外法相比也具有良好的相关性（r = 0.88）。基于分析结果和较短的运行时间，该方法适用于支持对接受治疗患者的人血清进行治疗药物监测的常规分析或药代动力学研究。
