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目的建立测定人血浆和尿液中吡西卡尼的高效液相色谱质谱联用方法。方法以液液萃取法进行样品处理,以乙腈-乙酸铵(0.1‰甲酸)-水为流动相(血药浓度测定:25∶37.5∶37.5;尿液中药物浓度测定:35∶6∶59),等度洗脱,经Welch Material Ultimate AQ-C18(2.1 mm×100 mm,3.5μm)色谱柱分离,流速0.35 mL·min-1、柱温25℃、进样量5μL。电喷雾离子源,正离子模式,多反应监测扫描(MRM),用于定量分析的离子反应分别为m/z 273.4→110.2(吡西卡尼)和m/z 287.4→110.2(内标,甲基吡西卡尼)。结果本法测定吡西卡尼浓度的线性范围分别为1~1 200μg·L-1(血浆),1~150 mg·L-1(尿液),最低定量限分别为1μg·L-1(血浆),1 mg·L-1(尿液),相关系数r值在0.996 2~0.999 1之间,提取回收率,基质效应,批内、批间精密度均满足药物浓度测定要求。临床药动学研究中,应用此法测定了人血浆和尿液吡西卡尼的浓度。结论本方法简便、准确、灵敏度高、重现性好,可以满足药动学研究中药物浓度测定的要求。
OBJECTIVE To establish a HPLC-MS method for the determination of piceatan in human plasma and urine. Methods The sample was processed by liquid-liquid extraction with acetonitrile-ammonium acetate (0.1 ‰ formic acid) -water as the mobile phase (blood concentration: 25:37.5:37.5; urine drug concentration: 35:6:59) , And eluted with isocratic elution. The sample was separated on a Welch Material Ultimate AQ-C18 column (2.1 mm × 100 mm, 3.5 μm) at a flow rate of 0.35 mL · min -1 and the column temperature was 25 ° C. Electrospray ionization, positive ion mode, multiple reaction monitoring and scanning (MRM), and ion reactions for quantitative analysis were m / z 273.4 → 110.2 (piracycline) and m / z 287.4 → 110.2 Pipirinide). Results The linear range of piracetam was 1 ~ 1 200 μg · L-1 (plasma) and 1 ~ 150 mg · L-1 (urine), the lowest limit of quantification was 1 μg · L-1 Plasma) and 1 mg · L-1 (urine). The correlation coefficient r was between 0.996 2 and 0.999 1. The extraction recovery, matrix effect, intra-assay and inter-assay precision all met the requirements of drug concentration determination. Clinical pharmacokinetic studies, the application of this method for the determination of human plasma and urine concentration of pi- Conclusion The method is simple, accurate, sensitive and reproducible, which can meet the requirements of drug concentration determination in pharmacokinetic studies.