Dziadosz Marek, Klintschar Michael, Teske Jörg
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Drug Metab Pers Ther. 2017 Sep 26;32(3):147-150. doi: 10.1515/dmpt-2017-0016.
As imatinib gained a lot of attention in the field of medicine, appropriate methods are needed for drug analysis. LC-MS/MS combined with complex sample preparation and column enrichment is usually the method of choice when high sensitivity is necessary. The application of LC-MS3 in imatinib quantification has not been discussed in the literature.
An LC-MS3 imatinib quantification method was developed and validated in human serum. The sample preparation was based on the liquid-liquid extraction of 50 μL human serum. Chromatographic separation was performed using a Luna 5 μm C18 (2) 100 A, 150 mm×2 mm column and the elution was done using a mobile phase consisting of A (H2O/methanol=95/5, v/v) and B (H2O/methanol=3/97, v/v), both with 10 mM ammonium acetate and 0.1% acetic acid.
The conditions applied resulted in a limit of detection/quantification value of 0.14/0.45 ng/mL reached without a sophisticated sample preparation technique or enrichment column application. It could be demonstrated that MS3 detection is a very effective way of sensitive imatinib quantification. Further, it could be stated that the strategy presented can be very useful for a sensitive analysis of other protein kinase inhibitors, because their molecule structure is appropriate for MS3 detection.
The presented analytical strategy is an effective way of protein kinase inhibitor analysis in human serum.
随着伊马替尼在医学领域备受关注,需要合适的药物分析方法。当需要高灵敏度时,液相色谱 - 串联质谱联用复杂的样品制备和柱富集通常是首选方法。液相色谱 - 质谱联用技术(LC-MS3)在伊马替尼定量分析中的应用尚未见文献报道。
建立了一种用于人血清中伊马替尼定量分析的LC-MS3方法并进行了验证。样品制备基于对50μL人血清的液 - 液萃取。色谱分离采用Luna 5μm C18(2)100A柱,柱长150mm×2mm,流动相由A(水/甲醇 = 95/5,v/v)和B(水/甲醇 = 3/97,v/v)组成,二者均含有10mM醋酸铵和0.1%乙酸。
所采用的条件在无需复杂样品制备技术或富集柱的情况下,检测限/定量限达到了0.14/0.45 ng/mL。结果表明,MS3检测是一种非常有效的伊马替尼灵敏定量分析方法。此外,可以说所提出的策略对于其他蛋白激酶抑制剂的灵敏分析可能非常有用,因为它们的分子结构适合MS3检测。
所提出的分析策略是一种用于人血清中蛋白激酶抑制剂分析的有效方法。