高效液相色谱法检查氯诺昔康中的有关物质及2-氨基吡啶

Determination of Related Substances and 2-aminopyridine in Lornoxicam by HPLC

目的：建立高效液相色谱法检查氯诺昔康的有关物质及有害物质2-氨基吡啶。方法：采用十八烷基键合硅胶色谱柱，以0.025mol·L-1磷酸二氢铵溶液（三乙胺调pH值至7.3）-甲醇（58：42）为流动相，流速为1.0ml·min-1，检测波长为290nm，柱温：30℃。结果：2-氨基吡啶、氯诺昔康主峰及各有关物质能够达到有效分离，方法耐用性良好，氯诺昔康检测限为2.006ng，2-氨基吡啶检测限为0.5045ng、定量限为1.009ng，2-氨基吡啶浓度在0.1009μg·mL-1～1.009μg·mL-1范围内线性关系良好（r=0.9997），2-氨基吡啶的平均回收率为106.5%（RSD=3.2%）。结论：本方法简便、稳定、专属性强，可用氯诺昔康有关物质及2-氨基吡啶的检查。

Objective：To establish an HPLC method to check lornoxicam related substances and hazardous material 2-aminopyr-idine. Methods：The C18 column was adopted with the mobile phase of 0.025 mol·L-1 ammonium dihydrogen phosphate solution-methanol （58：42） （triethylamine adjusted to pH 7.3） at the flow rate of 1.0 ml·min-1, and the detection wavelength was 290nm, column temperature：30℃. Results：2-aminopyridine, lornoxicam and relevant materials to achieve an effective separation method durability was good. The LOD of lornoxicam was 2.006ng, The LOD of 2-aminopyridine was 0.5045ng, The LOQ of 2-aminopyridine was 1.009 ng. The linear ranges of 2-aminopyridine was 0.100μg·mL-1~1.009μg·mL-1 （r=0.9997）. The average recovery of 2-amino-pyridine was 106.5%（RSD=3.2%）. Conclusion：The method was simple, stable, specific, and could be used lornoxicam related sub-stances, and 2-aminopyridine checks.