Clinical Pharmacology Research Center, Peking Union Medical College Hospital, Peking Union Medical College and Chinese Academy of Medical Sciences, Beijing 100032, China.
J Chromatogr B Analyt Technol Biomed Life Sci. 2013 Feb 1;915-916:28-32. doi: 10.1016/j.jchromb.2012.12.019. Epub 2012 Dec 26.
This paper described a sensitive and rapid method based on ultra-performance liquid chromatography coupled to tandem mass spectrometry (UPLC-MS/MS) for the determination of phenylephrine in human plasma. Plasma samples were pre-purified by solid-phase extraction (SPE). The chromatographic separation was achieved with BEH HILIC column using a mixture of 10mM pH 3.5 ammonium formate and acetonitrile (10:90, v/v) under isocratic conditions at a flow rate of 0.4 mL/min. The mass spectrometry was carried out using positive electrospray ionization (ESI) and data acquisition was carried out in the multiple reaction monitoring (MRM) mode. The method was fully validated over the concentration range of 10.0-5000 pg/mL. The lower limit of quantification (LLOQ) was 10.0 pg/mL. Inter- and intra-batch precision was less than 15% and the accuracy was within 85-115%. Extraction recovery was 78.5%. Selectivity, matrix effects and stability were also validated. The method was applied to the pharmacokinetic study of phenylephrine hydrochloride in Chinese subjects.
本文描述了一种基于超高效液相色谱-串联质谱（UPLC-MS/MS）的灵敏、快速测定人血浆中苯肾上腺素的方法。血浆样品经固相萃取（SPE）预净化。采用 BEH HILIC 柱，在 10mM pH 3.5 甲酸铵和乙腈（10:90，v/v）的混合溶液中，以 0.4 mL/min 的流速进行等度洗脱，实现色谱分离。质谱采用正电喷雾电离（ESI），数据采集采用多反应监测（MRM）模式。该方法在 10.0-5000 pg/mL 的浓度范围内进行了全面验证。定量下限（LLOQ）为 10.0 pg/mL。批内和批间精密度均小于 15%，准确度在 85-115%范围内。提取回收率为 78.5%。还验证了选择性、基质效应和稳定性。该方法应用于盐酸苯肾上腺素在中国受试者中的药代动力学研究。
