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目的:建立测定替诺福韦十八烷氧乙基单酯衍生物(ODE-TFV)中十八烷氧乙醇(ODE)含量的高效液相色谱-电喷雾检测器(HPLC-CAD)的方法。方法:采用Agilent ZORBAX XDB-C8柱(4.6 mm×75 mm,3.5μm),以0.1 mol·L-1醋酸铵缓冲液(pH 4.0)为流动相A,乙腈为流动相B,梯度洗脱,流速约为1.0 mL·min-1,柱温40℃;采用电喷雾检测器(charged aerosol detector,CAD),雾化室温度30℃,采样频率10 Hz;进样量10μL。结果:本法的线性范围为0.1000~10.00μg·mL-1(r=0.9999,n=6),最低检测限为50.00 ng·mL-1;最低定量限为100.0 ng·mL-1;方法平均回收率(n=9)为99.8%。结论:本文建立的方法能满足ODE-TFV原料药中ODE残留量监控的需要。
OBJECTIVE: To establish a high performance liquid chromatography-electrospray ionization detector (HPLC-CAD) method for the determination of octadecyl alcohol (ODE) in tenofenoxyethylene monoester derivative (ODE-TFV) . Methods: Agilent ZORBAX XDB-C8 column (4.6 mm × 75 mm, 3.5 μm) was used. The mobile phase A was consisted of 0.1 mol·L-1 ammonium acetate buffer (pH 4.0) The flow rate was about 1.0 mL · min-1 and the column temperature was 40 ℃. The sampling temperature was 10 Hz and the injection volume was 10 μL using a charged aerosol detector (CAD). Results: The linear range of this method was 0.1000-10.00μg · mL-1 (r = 0.9999, n = 6), the lowest limit of detection was 50.00 ng · mL-1 and the lowest limit of quantification was 100.0 ng · mL-1. The recovery (n = 9) was 99.8%. Conclusion: The method established in this paper can meet the need of ODE residue monitoring in ODE-TFV APIs.