Miura Masatomo, Takahashi Naoto, Sawada Ken-ichi
Department of Pharmacy, Akita University Hospital, 1-1-1 Hondo, Akita 010-8543, Japan.
J Chromatogr Sci. 2011 May;49(5):412-5. doi: 10.1093/chromsci/49.5.412.
A simple and sensitive high-performance liquid chromatography (HPLC) method was developed to quantitate imatinib in human plasma. Imatinib and the internal standard dasatinib were separated using a mobile phase of 0.5% KH(2)PO(4) (pH3.5)-acetonitrile-methanol (55:25:20, v/v/v) on a CAPCELL PAK C18 MG II column (250 mm × 4.6 mm) at a flow rate of 0.5 mL/min and measurement at UV 265 nm. Analysis required 100 μL of plasma and involved a solid phase extraction with an Oasis HLB cartridge, which gave recoveries of imatinib from 73% to 76%. The lower limit of quantification for imatinib was 10 ng/mL. The linear range of this assay was between 10 and 5000 ng/mL (regression line r(2) > 0.9992). Inter- and intra-day coefficients of variation were less than 11.9% and accuracies were within 8.3% over the linear range. The plasma concentrations of imatinib obtained by our present method were almost the same as those assayed by an LC-MS-MS method at the Toray Research Center, Inc. This method can be applied effectively to measure imatinib concentrations in clinical samples.
开发了一种简单灵敏的高效液相色谱（HPLC）方法来定量测定人血浆中的伊马替尼。伊马替尼和内标达沙替尼在CAPCELL PAK C18 MG II柱（250 mm×4.6 mm）上，以0.5%KH₂PO₄（pH3.5）-乙腈-甲醇（55:25:20，v/v/v）为流动相，流速为0.5 mL/min，在265 nm波长处进行紫外检测，实现分离。分析需要100 μL血浆，采用Oasis HLB柱进行固相萃取，伊马替尼的回收率为73%至76%。伊马替尼的定量下限为10 ng/mL。该检测方法的线性范围为10至5000 ng/mL（回归线r²>0.9992）。在整个线性范围内，日间和日内变异系数均小于11.9%，准确度在8.3%以内。通过我们目前的方法获得的伊马替尼血浆浓度与东丽研究中心采用LC-MS-MS方法测定的浓度几乎相同。该方法可有效应用于临床样本中伊马替尼浓度的测定。
