Clinical Pharmacology Research Center, Peking Union Medical College Hospital and Chinese Academy of Medical Sciences, Beijing 100730, China.
J Pharm Biomed Anal. 2012 Mar 5;61:237-41. doi: 10.1016/j.jpba.2011.10.022. Epub 2011 Oct 25.
A sensitive and selective high-performance liquid chromatography-tandem mass spectrometry (HPLC-MS/MS) method was developed to determine the cinacalcet hydrochloride in human plasma. The analyte was extracted from plasma samples using a 96-well plate automatic solid-phase extraction (SPE) device and chromatographed on an Inertsil SIL-150 (2.1 mm × 50 mm, i.d. 5 μm) column using acetonitrile-water-formic acid (90:10:1) as the mobile phase with an isocratic flow rate of 0.35 mL/min. The detection was performed on a triple quadrupole tandem mass spectrometer in multiple reaction monitoring (MRM) mode using positive electrospray ionization (ESI). The method was validated over the concentration range of 0.1-25 ng/mL. The indicators of inter- and intra-day precision (RSD%) were all within 15.1%, and the accuracy (RE%) was within ± 15%. The lower limit of quantitation (LLOQ) was 0.1 ng/mL. The average extraction recovery was 51.7%, and the detection was not affected by the matrix. The method was successfully applied to a pharmacokinetic study of cinacalcet hydrochloride in healthy Chinese volunteers.
建立了一种灵敏、选择性的高效液相色谱-串联质谱（HPLC-MS/MS）法，用于测定人血浆中的盐酸西那卡塞。采用 96 孔板自动固相萃取（SPE）装置从血浆样品中提取分析物，采用 Inertsil SIL-150（2.1mm×50mm，内径 5μm）柱，以乙腈-水-甲酸（90:10:1）为流动相，等度洗脱，流速为 0.35mL/min。采用正电喷雾电离（ESI），在三重四极杆串联质谱仪上以多反应监测（MRM）模式进行检测。该方法在 0.1-25ng/mL 的浓度范围内进行了验证。日内和日间精密度（RSD%）的各项指标均在 15.1%以内，准确度（RE%）在±15%以内。定量下限（LLOQ）为 0.1ng/mL。平均提取回收率为 51.7%，且检测不受基质影响。该方法成功应用于盐酸西那卡塞在中国健康志愿者中的药代动力学研究。
