HPLC法测定氯诺昔康片中有关物质的含量

Content Determination of the Related Substances in Lornoxicam Tablets by HPLC

目的:建立测定氯诺昔康片有关物质含量的方法。方法:采用高效液相色谱法。色谱柱为Thermo Hypersil ODS,流动相A为1%醋酸铵溶液-10%氢氧化四丁基铵溶液-甲醇(1 000∶6.4∶4.4),流动相B为乙腈-辛胺(99.9∶0.1),梯度洗脱,流速为0.5ml/min,可变波长检测器,检测波长为280 nm,柱温为35℃。测定3批样品中4种已知杂质2-氨基吡啶、HN-40244、HN-10004、HN-10002及其他单个杂质和总杂质含量。结果:4种已知杂质以及其他单个杂质均能与氯诺昔康完全分离,4种已知杂质在各自的检测质量浓度范围内线性关系良好(r≥0.999 8),检测限分别为0.64、0.28、0.29、0.24 ng,定量限分别为1.30、0.93、0.95、0.40ng。结论:建立的方法结果准确,可全面检测氯诺昔康片中有关物质的含量。

OBJECTIVE： To establish a method for the content determination of the related substances in Lomoxicam tablets. METHODS： HPLC method was adopted. The determination was performed on Thermo Hypersil ODS column with 1% ammonium acetate solution-10% tetrabutyla mmonium hydroxide solution-methanol （1 000：6.4：4.4） as the mobile phase A and acetonitrile-oc- tylamine （99.9：0.1） as mobile phase B （gradient elution）. The flow rate was 0.5 ml/min and the column temperature was 35 ~2. The detection wavelength of VWD detector was set at 280 nm. The contents of 4 kinds of known impurity （2-amino pyridine, HN- 40244, HN-10004 and HN-10002）, other single impurity and total impurity were all determined in 3 batches of samples. RESULTS： 4 kinds of known impurities and other single impurity were all separated from lornoxicam completely. There was a good linear rela- tionship between calibration curve and the concentration of 4 kinds of known impurities （r〉0.999 8）. The limits of detection were 0.64,0.28, 0.29 and 0.24 ng, respectively. The limits of quantification were 1.30 ng, 0.93 ng, 0.95 ng and 0.40 ng, respectively. CONCLUSIONS： The method is accurate and suitable for the content determination of the related substances in Lomoxicam tablets.