高效液相色谱法测定盐酸多西环素可溶性粉的含量

Determination of Doxycycline Hyclate Powder

关键词:  高效液相色谱法  盐酸多西环素可溶性粉  含量测定

Key words:  HPLC  doxycycline hyclate powder  determination

摘要:

目的：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，并对检验方法进行复核验证。方法[1]：色谱柱 Waters Nova.pak®C18( 3.9mm×150mm， 4μm)；以0.05mol/L草酸铵溶液-二甲基甲酰胺-0.2mol/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℃；检测波长为280nm；流速1.0mL/min；进样量为20μL。结果：多西环素进样浓度在4.0～144.0μg/mL的范围内与峰面积呈良好的线性关系（r=1.000 0）；样品的平均加样回收率（n=9）为98.5%，RSD为2.0%；我们完成了185批次样品的检验，检验结果准确可靠。结论：该法准确度高，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。

Abstract:

To detect the contents of doxycycline in doxycycline hyclate powder using high performance liquid chromatography and re-validate the determination. Method[1] : Column Waters Nova.pak®C18( 3.9mm×150mm , 4μm) with 0.05mol/L diammonium oxalate —N,N-dimethylfromamide —0.2mol/mL diammonium dydrogen phosphate（65:30:5）(using diammonium charge to regulate the pH value to 8.0) was used as mobile phase. The column temperature was 35℃. The detection wavelength was 280nm. The flow rate was 1.0mL/min. The injection volume was 20μL. Results: There was a good linear correlation between the peak areas and the concentrations of doxycycline and the range from 4.0～144.0μg/mL( r=1.000 0). The average recovery was 98.5% and RSD was 2.0%.We have detected 185 samples and the results were accurate and reliable. Conclusion:The results indicated that the constructed method was accurate, repeatable and reliable.