摘要
目的建立快速检测大鼠血浆中伊马替尼浓度的UPLC-MS/MS方法。方法用乙腈沉淀血浆蛋白的方法处理,运用三重四级杆液质联用仪,色谱柱为CORTECS^(TM)UPLC~C18柱(100 mm×2.1 mm,1.6μm);流动相为乙腈-水(含0.1%甲酸),梯度洗脱,流速为0.4 ml·min^(-1),柱温40℃,内标为阿帕替尼;质谱条件:电喷雾离子化源(ESI),正离子检测模式。结果伊马替尼的保留时间为0.94 min,线性范围为10~1600 ng·ml^(-1)(r=0.9991),最低定量限为2 ng·ml^(-1),回收率为73.91%~77.88%,日内、日间RSD均<10%。结论该法准确可靠,操作简便,重复性好,适于检测大鼠血浆中伊马替尼的浓度。
Objective To establish an ultra performance liquid chromatography-tandem quadrupole mass spectrometry method for the determination of imatinib in rat plasma. Methods A CORTECS^TMUPLC^(R)C_(18)( 100 mm ×2. 1 mm,1. 6 μm) column was used as the stationary phase at 40 ℃. The mobile phase consisted of acetonitrile and water( containing 0. 1% formic acid) at gradient elution pumped at a flow rate of 0. 4 ml·min^-1. The analytes were detected on a triple-quadrupole mass spectrometer equipped with an ESI interface in a positive mode. Results The retention time of imatinib was 0. 94 min. Excellent linear calibration curves of imatinib were obtained in the concentration range of 10- 1600 ng·ml^-1( r =0. 9991). The lower limit of quantification of imatinib was 2 ng·ml^-1 while the average recovery was 73. 91%- 77. 88%. The intra and inter day six standard deviations were below 10%. Conclusion This method is accurate,simple and suitable for the determination of imatinib in rat plasma.
出处
《解放军药学学报》
CAS
CSCD
2015年第6期473-476,480,共5页
Pharmaceutical Journal of Chinese People's Liberation Army
基金
国家自然科学基金青年科学基金项目
No.81401558