高效液相色谱法分离测定奥柳氮钠及其杂质

Separation and Determination of Olsalazine Sodium and Its Impurities by HPLC

目的 :用反相离子对高效液相色谱法分离测定奥柳氮钠及其相关物质。方法 :采用AlltimaC18色谱柱 ,以甲醇 -离子对缓冲液 (含 0 0 2mol·L-1磷酸二氢钠和 0 0 2mol·L-1四乙基氢氧化铵 ,pH 7 2 ) (4 5∶5 5 )为流动相 ,流速 1 0mL·min-1,检测波长 340nm。结果 :奥柳氮钠在 2 0～ 12 5 μg·mL-1线性良好 ,并能有效分离合成中间体和副产物。结论 :该法简便 ,结果准确 ,能有效控制产品质量。

Objective:A reversed phase HPLC method was described for separation and determination of olsalazine sodium and its impurities.Methods:The analysis was achieved by using Alltima C 18 column with methanol-ion\|pair buffer solution (45∶55) as mobile phase and UV-detector at wavelength 340 nm.The flow rate was 1 0 mL·min -1 . The ion-pair buffer solution was a mixture of 0 02 mol·L -1 sodium dihydrogen phosphate and 0 02 mol·L -1 tetraethylammonium hydroxide adjusted pH 7 2 with phosphoric acid.Results:The linear range of calibration curve was 20～125 μg·mL -1 ( r= 0 999 9) and the detection limits was l ng ( S/N >3).The results of assay for three batches of sample were 99 8%,100 5%,99 7%,and of impurities were 0 67%,0 62%,0 86% respectively.The identification of impurities was showed that one of impurities was the product caused by side-reaction during synthesis.Conclusion:The method is simple,accurate and can be used to control the quality.