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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LunaTMC8色谱柱(2.00 mm×150 mm,3μm)分离,以乙腈-0.3 mmol·L-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 mL·min-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 ng·mL-1内线性关系良好,定量下限为3 ng·mL-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 establish a liquid chromatography-tandem mass spectrometry (LC-MS / MS) method for the determination of pinacidol in human urine and investigate its urine excretion in Chinese healthy subjects. Methods Urine samples were separated by liquid-liquid extraction with ether and separated on a LunaTMC8 column (2.00 mm × 150 mm, 3 μm). The mobile phase was acetonitrile-0.3 mmol·L-1 ammonium acetate aqueous solution (65:35, V / V) Isocratic elution at a flow rate of 0.25 mL · min-1 was performed by electrospray ionization (ESI) and multiple reaction monitoring (MRM) negative ion mode. Eight subjects were given intravenous nitinarine 40 mg to determine urinary excretion parameters of pinocitinin. Results Pinosin was linear in the concentration range of 3 ~ 200 ng · mL-1 with a lower limit of quantification of 3 ng · mL-1. The intra-assay and inter-assay variation (RSD) was less than 6.34% and the stability was good. After administration of the test substance, the cumulative urinary excretion rate of pinacidol at 4 h after the administration reached the platform, and the cumulative excretion rate at 48 h was (0.11 ± 0.05)%. Conclusion The method is rapid, sensitive, accurate, specific and reproducible. It is suitable for the determination of pinacidol in human urine and the study of urinary excretion.