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目的建立人血浆中普瑞巴林含量测定的液相色谱串联质谱方法,并用于癫痫患者的血药浓度测定。方法色谱柱:Diamonsil C_(18)柱(150 mm×4.6mm,5μm),流动相:甲醇-水(0.05%甲酸),梯度洗脱流量:1 mL·min~(-1),进样量:20μL,柱温:30℃。用电喷雾离子源进行正离子模式监测,用多反应监测模式(MRM)进行定量分析,源喷射电压为5500 V,离子源温度为650℃。考察该方法的专属性、标准曲线、检测限、精密度、回收率及稳定性。选取20名门诊癫痫患者,第1次口服普瑞巴林胶囊75 mg 1 h后,采静脉血,用HPLC-MS/MS法测定普瑞巴林的血药浓度。结果普瑞巴林在13.76~5270.00 ng·mL~(-1)内线性关系良好,最低定量下限为0.65 ng·mL~(-1)。平均回收率在94%以上,日间、日内精密度RSD值均小于15%,稳定性良好。用该方法测定20名癫痫患者血样,其血药浓度范围为1.76~2.78μg·mL~(-1)。结论本法简便、快速、灵敏度高、专属性好,可用于癫痫患者普瑞巴林血药浓度的测定。
Objective To establish a method for the determination of pregabalin in human plasma by liquid chromatography-tandem mass spectrometry (HPLC-MS / MS) and to determine the concentration of pregabalin in human plasma. Methods Column: Diamonsil C_ (18) column (150 mm × 4.6 mm, 5 μm) with mobile phase of methanol-water (0.05% formic acid) and gradient elution flow rate of 1 mL · min -1 : 20 μL, column temperature: 30 ° C. Positive ion mode monitoring was performed with an electrospray ion source and quantitatively analyzed using a multiple reaction monitoring mode (MRM) with a source injection voltage of 5500 V and an ion source temperature of 650 ° C. Investigate the specificity of the method, the standard curve, detection limit, precision, recovery and stability. 20 outpatients with epilepsy were selected. After the first oral administration of pregabalin capsules 75 mg for 1 h, venous blood was collected and the plasma concentration of pregabalin was determined by HPLC-MS / MS. Results Pregabalin showed a good linearity within the range of 13.76 ~ 5270.00 ng · mL -1 with the lowest limit of quantitation of 0.65 ng · mL -1. The average recovery rate was above 94%. The RSD values were less than 15% during the day and the day, and the stability was good. Blood samples of 20 patients with epilepsy were measured by this method. The range of plasma concentration was 1.76 ~ 2.78μg · mL ~ (-1). Conclusion The method is simple, rapid, sensitive and specific. It can be used for the determination of pregabalin in patients with epilepsy.