摘要
目的建立测定白消安血药浓度的HPLC-MS/MS分析方法。方法血浆中加入白消安-d8作为内标,以乙腈提取,进行HPLC-MS/MS的测定。采用Agilent ZORBA SB-C18色谱柱（150mm×4.6mm,5μm）,以10mmol·L^-1乙酸铵缓冲液∶甲醇（60∶40）作为流动相,流速：0.5m L·min^-1,柱温：35℃,进样量：10μL;质谱条件：采用电喷雾离子源（ESI）四级杆质谱,以选择性离子监测方式（SIM）进行正离子检测。结果白消安的线性范围为0.0206~10.2826μmol·L^-1,标准曲线为y=1.148x＋5.400×10-2,r=0.9980,低、中、高3个浓度质控样品日内和日间RSD均〈15%,平均提取回收率为94.26%。结论该方法准确、灵敏、快速,已成功应用于白消安血药浓度的测定及其体内药动学分析。
OBJECTIVE To established an analysis method to determine Busulfan plasma concentration by liquid chromatography-tandem mass spectrometry（HPLC-MS/MS）. METHODS Busulfan in human plasma was extracted by 1acetonitrle,with Busulfan-d8 as internal standard. The samples were separated by Agilent ZORBA SB-C18column（150 mm × 4. 6mm,5μm）,the mobile phase consisted of 10 mmol · L^-1ammonium acetate ∶ methanol（60 ∶40）,as flow rate of 0. 5m L·min^-1,column temperature： 35℃,injection volume： 10μL. Mass spectrometry conditions：triple-quadrupole mass spectrometry with electrospray ion source,positive ion detection in selective ion monitoring mode. RESULTS The linear range of busulfan was 0. 0206- 10. 2826μmol · L^-1,the standard curve is Y =0. 008 X ＋ 0. 011,r = 0. 96,the intra-and inter-day RSDs were all below 15% at low,moderate and high concentrations. The mean extract recoveries were 94. 26%. CONCLUSION The method is accurate,sensitive,fast,and is suitable for the determination of Busulfan plasma drug concentration and its pharmacokinetic analysis.
出处
《海峡药学》
2014年第11期243-246,共4页
Strait Pharmaceutical Journal
基金
福建省战略新兴技术应用项目(2013J01371)
