目的 建立高效液相色谱-串联质谱(LC-MS/MS)测定人尿中匹诺塞林浓度,考察其在中国健康受试者尿液中的排泄特征。方法 尿样用乙醚液-液萃取,采用Luna^TMC₈色谱柱(2.00 mm×150 mm,3 μm)分离,以乙腈-0.3 mmolL^-1醋酸铵水溶液(65∶35, V/V)为流动相进行等度洗脱,流速为0.25 mLmin^-1,通过电喷雾离子源(ESI),多重反应监测(MRM)负离子模式进行检测。8名受试者静脉滴注匹诺塞林40 mg,测定匹诺塞林的尿药排泄参数。结果 匹诺塞林在3~200 ngmL^-1内线性关系良好,定量下限为3 ngmL^-1,批内、批间变异(RSD)小于6.34%,稳定性较好。受试者给药后,匹诺塞林在给药结束后4 h尿的累积排泄百分率达到平台,48 h累计排泄百分率为(0.11±0.05)%。结论 该方法快速、灵敏、准确、专属性强、重现性高,适用于人尿中匹诺塞林的测定及其尿药排泄特征研究。

OBJECTIVE To develop a liquid chromatography-tandem mass spectrometry (LC-MS/MS) method for determination of pinocembrin in human urine, and to investigate its urinary excretory after intravenous drip administration of pinocembrin in healthy volunteers. METHODS The urine samples were extracted with ether. The separation was performed on a Luna C₈ column (2.00 mm×150 mm, 3 μm) using the mobile phase composed of acetonitrile-0.3 mmolL^-1 ammonium acetate solution (65∶35, V/V) at a flow rate of 0.25 mLmin^-1 in isocratic mode. The detection was performed on a triple quadrupole tandem mass spectrometer by multiple reaction monitoring (MRM) via electrospray ionization (ESI) source in negative mode. Urinary excretion parameters were calculated after a single intravenous drip administration of pinocembrin at 40 mg to humans. RESUTLS The assay was linear from 3 ngmL^-1 to 200 ngmL^-1, with the lower limit of quantification at 3 ngmL^-1. The within-run and between-run precision (RSD) were below 6.34%. Pinocembrin had good stability. At 4 h after the completion of administration, the urinary cumulative excretion percentage reached a plateau and the cumulative excretion percentage in urine within 48 h were (0.11±0.05) %. CONCLUSION This method is rapid,sensitive, accurate, specific and reliable, and suitable for the determination of pinocembrin in human urine and for the investigation to the urinary excretion.