Pirro Elisa, De Francia Silvia, De Martino Francesca, Fava Carmen, Ulisciani Stefano, Cambrin Giovanna Rege, Racca Silvia, Saglio Giuseppe, Di Carlo Francesco
Clinical Pharmacology, Clinical and Biological Sciences Department, University of Turin, S. Luigi Hospital, Orbassano, TO, Italy.
J Chromatogr Sci. 2011 Nov-Dec;49(10):753-7. doi: 10.1093/chrsci/49.10.753.
Development and validation of simple, rapid, and reliable high-performance liquid chromatography (HPLC)-UV method for quantification of major tyrosine kinase inhibitors, imatinib, dasatinib, and nilotinib, in human plasma is presented. Chromatographic separation of the drugs is achieved on an RP-C(18) column at flow rate of 0.9 mL/min at 35°C; eluate is monitored at 267 nm. Mean intra-day and inter-day precision for all compounds are 2.5 and 13.3%; mean accuracy is 13.9%; extraction recovery ranges within 40.24 and 81.81%. Calibration curves range from 10 to 0.005 μg/mL. Limits of detection are 10 ng/mL for imatinib and nilotinib, 50 ng/mL for dasatinib; limits of quantitation are 50 ng/mL for imatinib and nilotinib, 100 ng/mL for dasatinib. Although this method allows the detection of dasatinib, levels found in patients plasma are close to the limit of detection, then below the limit of quantitation. Quantification with HPLC-mass spectrometry, then, is required for dasatinib to give a correct evaluation. In conclusion, the sensitivity of this new method is sufficient to perform therapeutic monitoring and pharmacokinetic studies of imatinib and nilotinib but not dasatinib in CML patients.
本文介绍了一种简单、快速且可靠的高效液相色谱(HPLC)-紫外检测法的开发与验证,用于定量测定人血浆中主要的酪氨酸激酶抑制剂伊马替尼、达沙替尼和尼洛替尼。药物的色谱分离在RP-C(18)柱上进行,柱温35°C,流速0.9 mL/min;在267 nm处监测洗脱液。所有化合物的日内和日间平均精密度分别为2.5%和13.3%;平均准确度为13.9%;萃取回收率在40.24%至81.81%之间。校准曲线范围为10至0.005 μg/mL。伊马替尼和尼洛替尼的检测限为10 ng/mL,达沙替尼的检测限为50 ng/mL;伊马替尼和尼洛替尼的定量限为50 ng/mL,达沙替尼的定量限为100 ng/mL。虽然该方法能够检测到达沙替尼,但在患者血浆中检测到的水平接近检测限,低于定量限。因此,对于达沙替尼,需要采用HPLC-质谱法定量才能进行正确评估。总之,这种新方法的灵敏度足以对慢性粒细胞白血病患者的伊马替尼和尼洛替尼进行治疗监测和药代动力学研究,但对达沙替尼则不适用。