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目的:建立同时测定人血浆中伊马替尼及伏立康唑浓度的高效液相色谱法。方法:血桨样品经乙酸乙酯-正己烷(75:25)萃取,选择卡马西平为内标,氮吹浓缩、复溶后采用HPLC分析。ZORBAX SB-C18柱反相柱(250 mm×4.6 mm,5 mm)为色谱柱,流动相为甲醇-乙腈-醋酸铵缓冲液(25 mmol·L~(-1) CH_3COONH_4,CH_3COOH调pH值至4.5)=20:32:48(V/V/V),检测波长264 nm,流速为1 mL·min~(-1),柱温35℃,进样量为20μL。结果:伊马替尼、伏立康唑血药浓度线性范围分别为0.10-5.00μg·mL~(-1)和0.10-6.00μg·mL~(-1),两者的线性均良好(r分别为0.998和0.999),最低定量下限均为0.10μg·mL~(-1)。伊马替尼和伏立康唑低、中、高质量浓度的提取回收率分别为69.21%,71.23%,73.53%和76.23%,78.12%,79.34%,二者批内RSD均小于15%。结论:该方法简便、快速、灵敏度高可满足同时检测伊马替尼和伏立康唑的临床血药浓度监测及药动学研究。
Objective: To establish a HPLC method for the simultaneous determination of imatinib and voriconazole in human plasma. METHODS: Blood samples were extracted with ethyl acetate-n-hexane (75:25). Carbamazepine was selected as internal standard and concentrated by nitrogen. The reconstituted samples were analyzed by HPLC. The mobile phase consisted of methanol-acetonitrile-ammonium acetate buffer (25 mmol·L -1 CH_3COONH_4) and CH_3COOH adjusted to pH = 4.5) = 20:32:48 (V / V / V). The detection wavelength was set at 264 nm and the flow rate was 1 mL · min -1. The column temperature was 35 ℃ and the injection volume was 20 μL. Results: The linear ranges of imatinib and voriconazole were 0.10-5.00μg · mL -1 and 0.10-6.00μg · mL -1, respectively, with good linearity (r = 0.998 And 0.999), the lowest limit of quantification was 0.10μg · mL -1. The recovery rates of imatinib and voriconazole at low, middle and high concentrations were 69.21%, 71.23%, 73.53% and 76.23%, 78.12% and 79.34%, respectively. The intra-assay RSDs were both less than 15%. Conclusion: The method is simple, rapid and sensitive and can meet the need of simultaneous monitoring of imatinib and voriconazole in clinical plasma concentration monitoring and pharmacokinetics.