Clinical Pharmacy, Necker Hospital, 149 rue de Sèvres, Paris 75015, France.
Hematology Department, Necker Hospital, 149 rue de Sèvres, Paris 75015, France; Centre de référence des mastocytoses (CEREMAST), Necker Hospital, 149 rue de Sèvres, Paris 75015, France.
J Chromatogr B Analyt Technol Biomed Life Sci. 2014 Jan 1;944:175-81. doi: 10.1016/j.jchromb.2013.11.003. Epub 2013 Nov 15.
We developed and validated quantitative bioanalytical liquid chromatography-tandem mass spectrometry assay for the protein kinase inhibitor, midostaurin. Plasma samples were pre-treated using a protein precipitation with methanol containing midostaurin-d5 as an internal standard. After centrifugation, 5μL of the supernatant was injected into the chromatographic system. The system consisted of a 3.5μm particle bonded octadecyl silica column, with gradient elution using a mixture of 0.1% (v/v) formic acid in acetonitrile and 10mM ammonium formate in water with 0.1% formic acid. The analyte was quantified using the selected reaction-monitoring mode of a triple quadrupole mass spectrometer equipped with a heated electrospray interface. The assay was validated in a 75-2500ng/mL calibration range. For quality control, within-day and between-day precisions were 1.2-2.8%, and 1.2-6.9%, respectively. The β-expectation tolerance limit (accuracy) met the limits of acceptance ±15% (±20% for the LLQ). The drug was sufficiently stable under all relevant analytical conditions. The assay has successfully been used to assess drug levels for therapeutic drug monitoring in patients presenting advanced systemic mastocytosis and treated with the promising midostaurin.
我们开发并验证了一种用于蛋白激酶抑制剂米哚妥林的定量生物分析液相色谱-串联质谱检测法。采用含米哚妥林-d5 的甲醇进行蛋白沉淀预处理血浆样品作为内标。离心后,取 5μL 上清液注入色谱系统。系统采用 3.5μm 颗粒键合十八烷基硅烷柱,以含 0.1%(v/v)甲酸的乙腈和含 10mM 甲酸铵的水的混合物为流动相进行梯度洗脱,甲酸的浓度为 0.1%。采用配备加热电喷雾接口的三重四极杆质谱仪的选择反应监测模式定量分析分析物。该测定法在 75-2500ng/mL 的校准范围内进行了验证。对于质控,日内和日间精密度分别为 1.2-2.8%和 1.2-6.9%。β-期望公差限值(准确度)符合接受限±15%(对于低限,接受限为±20%)。在所有相关分析条件下,药物均稳定。该检测法已成功用于评估接受有前景的米哚妥林治疗的晚期系统性肥大细胞增多症患者的治疗药物监测中的药物水平。