The contents of doxycycline in doxycycline hyclate powder were detected by high performance liquid chromatography and the determination was re-validated. Column Waters Nova.pakR○C18(3.9 mm×150 mm,4 μm) with 0.05 mol/L diammonium oxalate -N,N-dimethylfromamide -0.2 mol/mL diammonium dydrogen phosphate(65∶30∶5)(pH 8.0 regulated with diammonium) was used as mobile phase. The column temperature was 35 ℃. The detection wavelength was 280 nm. The flow rate was 1.0 mL/min. The injection volume was 20 μL. There was a good linear correlation between the peak areas and the concentrations of doxycycline and the range from 4.0～144.0 μg/mL( r=1.000). The average recovery was 98.5% and RSD was 2.0%(n=9).185 samples had been detected and the results were accurate and reliable. The results indicated that the constructed method was accurate, repeatable and reliable.%采用高效液相色谱法(HPLC)测定盐酸多西环素可溶性粉中多西环素的含量,并对检验方法[1]进行复核验证.色谱柱 Waters Nova.pakR○C18( 3.9 mm×150 mm, 4 μm);以0.05 mol/L草酸铵溶液-二甲基甲酰胺-0.2 mol/L磷酸氢二铵溶液(65∶30∶5)(用氨试液调节pH值为8.0)为流动相;柱温35 ℃;检测波长280 nm;流速1.0 mL/min;进样量20 μL.多西环素进样浓度在4.0～144.0 μg/mL的范围内与峰面积呈良好的线性关系(r=1.000);样品的平均加样回收率(n=9)为98.5%,RSD为2.0%;完成了185批次样品的检验,检验结果准确可靠.该方法准确度高,重复性好,结果可靠,能够有效地检测盐酸多西环素可溶性粉的含量.
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