摘要
目的:采用高效液相色谱-串联质谱法(HPLC-MS/MS)建立测定人血浆中尼洛替尼浓度的检测方法。方法:血样经甲醇除蛋白后,流动相分别为0.1%甲酸的甲酸铵缓冲液(A相)和0.1%甲酸的乙腈溶液(B相)梯度洗脱,LunaC_(18)柱(20 mm×2.0 mm,3μm)色谱柱分离,流速为0.6 ml·min^(-1);柱温35℃;电喷雾离子源(ESI),正离子模式,多反应监测,离子对为m/z 530.1→m/z 288.9(尼洛替尼)、m/z 502.3→m/z 394.1(伊马替尼-D8)。结果:尼洛替尼的线性范围为50~10000 ng·ml^(-1),定量下限为50 ng·ml^(-1);日内及日间RSD均小于10%,尼洛替尼低、中、高浓度的提取回收率分别为98.5%,102.4%,103.3%。结论:本检测方法操作简单、灵敏度高、检测下限低、专属性强,适用于临床慢性髓系白血病(CML)患者血浆中尼洛替尼的检测。
Objective:To establish a method for the determination of nilotinib in human plasma by HPLC-MS/MS.Methods:Plasma samples were precipitated by methanol.High performance liquid chromatographic separation was performed on a LunaC_(18) column(20 mm×2.0 mm,3μm)with 0.1%formic acid in both ammonium formate buffer solution and acetonitrile as the mobile phase in a gradient elution manner.The flow rate was 0.6 ml·min-1 and the column temperature was 35℃.Electrospray ionization(ESI)with a positive-ion and multiple reactions monitoring mode was adopted.The ion pairs were m/z 503.1→m/z 288.9 for nilotinib,and m/z 502.3→m/z 394.1 for imatinib-D8.Results:The linear range of nilotinib was 50-10000 ng·ml^(-1),and the lower limit of quantitation was 50 ng·ml^(-1);the intra-and inter-day relative standard deviations were lower than 10%.The extraction recoveries of low,medium and high concentration control samples were 98.5%,102.4%and 103.3%,respectively.Conclusion:The method has the advantages of simplicity,high sensitivity,low detection limit and strong specificity.It is suitable for the determination of nilotinib in chronic myeloid leukemia(CML)patients.
作者
程芳
李强
王静林
曾芳
黎纬明
张玉
Cheng Fang;Li Qiang;Wang Jinglin;Zeng Fang;Li Weiming;Zhang Yu(Department of Pharmacy,Union Hospital,Tongji Medical College,Huazhong University of Science and Technology,Wuhan 430022,China;Hubei Province Clinical Research Center for Precision Medicine for Critical Illness;Department of Hematology,Union Hospital,Tongji Medical College,Huazhong University of Science and Technology)
出处
《中国药师》
CAS
2022年第8期1379-1383,共5页
China Pharmacist
基金
湖北省重点研发计划项目(编号:2020BCA060)。
