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目的建立快速测定人血浆中帕洛诺司琼浓度的高效液相色谱串联质谱电喷雾检测(LC-ESI-MS/MS)法。方法以Aglent C_(18)反相柱(150 mm×4.6 mm,5μm)为色谱柱,流动相为乙腈:0.04 mol·L~(-1)甲酸铵水溶液(含0.04%甲酸)=80:20(V/V),流速0.8mL·min~(-1),柱温25℃,醋酸乙酯:二氯甲烷(4:1,V:V)为提取剂。样品经电喷雾离子源正离子化后,通过三重四级杆串联质谱仪,采用选择反应监测(SRM)模式对帕洛诺司琼(m/z 297.2→82.2)和内标地西泮(m/z285.1→154.0)进行测定。结果帕洛诺司琼高(8μg·L~(-1))、中(5μg·L~(-1))、低(0.1μg·L~(-1))3个质量浓度血浆溶液的RSD均<15%;线性范围为0.05～10μg·L~(-1),回归方程为F=1.831 9ρ+0.009 8,r=0.996 4(n=9),权重系数为1/ρ~2,分析方法的定量下限为0.05μg·L~(-1)。结论该方法灵敏、准确、简单、快速,可用于帕洛诺司琼临床血药浓度监测和药动学研究。
OBJECTIVE To establish a method for the rapid determination of palonosetron in human plasma by high performance liquid chromatography tandem mass spectrometry (LC-ESI-MS / MS). Methods Aglent C 18 column (150 mm × 4.6 mm, 5 μm) was used as the mobile phase. The mobile phase was acetonitrile: 0.04 mol·L -1 ammonium formate solution (containing 0.04% formic acid) = 80:20 (V / V), flow rate 0.8mL · min -1, column temperature 25 ℃, ethyl acetate: dichloromethane (4: 1, V: V) as extractant. The samples were ionized by electrospray ionization and analyzed by triple quadrupole tandem mass spectrometry (ESI-MS / MS) using selective reaction monitoring (SRM) mode for palonosetron (m / z 297.2 → 82.2) and internal standard diazepam /z285.1→154.0). Results The plasma concentrations of palonosetron (8μg · L -1), medium (5μg · L -1) and low (0.1μg · L -1) (P <0.05). The linear range was 0.05-10 μg · L -1, the regression equation was F = 1.831 9ρ + 0.009 8, r = 0.996 4 (n = 9) and the weight coefficient was 1 / ρ ~ 2 The lower limit of quantitation was 0.05 μg · L -1. Conclusion The method is sensitive, accurate, simple and rapid and can be used for the clinical monitoring of plasma concentration of palonosetron and pharmacokinetics.