高效液相色谱－电喷雾检测器测定ODE-TFV中ODE残留量
etermination of ODE in ODE-TFV by HPLC-CAD
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-电喷雾检测器的方法。方法：采用Agilent ZORBAX XDB-C8柱（4.6 mm×75 mm,3.5 μm），以0.1 moloL-1醋酸铵缓冲液(pH4.0)为流动相A，乙腈为流动相B，梯度洗脱；柱温40 ℃；流速约为1.0 mLomin-1；采用电喷雾检测器（CAD），雾化室温度30 ℃，采样频率10 Hz；进样量10 μL。结果：本法的线性范围为0.1~10 μgomL-1（r=0.9999，n=6），最低检测限为0.05 μgomL-1；最低定量限为0.1 μgomL-1；方法平均回收率为100.3%（n=9）。结论：该HPLC法灵敏、简便、准确、重现性好，能满足ODE-TFV原料药中ODE残留量监控的需要。
Objective: To establish the HPLC-CAD method for the determination of ODE in the sample of ODE-TFV. Methods: ODE-TFV and ODE were separated on a Agilent ZORBAX XDB-C8 column (4.6 mm×75 mm, 3.5 μm). The mobile phase was composed of 0.1 moloL-1 ammonium acetate buffer (pH4.0) and acetonitrile with gradient elution mode at a flow about 1.0 mLomin-1; CAD; nebulization temperature was 30 ℃ and collection frequency was 10 Hz; the injection volume was 10 μL and column temperature was 40 ℃. Results: The linear range of the method was 0.1-10 μgomL-1 (r=0.9999, n=6), the lowest limit of detection was 0.05 μgomL-1; LOQ was 0.1 μgomL-1; method of average recovery was 100.1%-100.5%. Conclusion: The HPLC method established is sensitive, simple, accurate, reproducible, and can meet the quality control requirements.?????
山广志、李卓荣、左利民、周洁、易红、姜宏
药学制药化学工业
药物分析ODE-TFVODE电喷雾检测器高效液相色谱法残留量
Pharmaceutical AnalysisODE-TFVODECADHPLCamount of residue
山广志,李卓荣,左利民,周洁,易红,姜宏.高效液相色谱－电喷雾检测器测定ODE-TFV中ODE残留量[EB/OL].(2014-02-26)[2025-08-10].http://www.paper.edu.cn/releasepaper/content/201402-503.点此复制
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