UPLC梯度洗脱法测定注射用阿洛西林钠中有关物质

UPLC gradient elution method for the determination of the related substances in azlocillion sodium for injection

目的 探索建立合适的超高效液相色谱-梯度洗脱法检测注射用阿洛西林钠的有关物质,采用LC-MS法对注射用阿洛西林钠的部分有关物质进行鉴定.方法 色谱柱为ACQUITY UPLC BEH C18,2.1mm×100mm,1.7mm;流动相A为10mmol/L甲酸铵溶液（用氨水调节pH值至6.5）,流动相B为8mmol/L甲酸铵溶液（乙腈/水=200/50）;柱温为40℃;检测波长为210hm;流速为0.43mL/min.结果 阿洛西林钠主峰与其相关物质峰分离良好,检出杂质数量远多于中国药典2010年版二部各论方法;在0.3～90μg/mL范围内阿洛西林呈良好的线性关系（r2=0.9999）,方法的检测限为0.1μg/mL,重复性RSD为0.61％（n=6）.结论 改进的UPLC方法的色谱性能明显优于现行标准方法,且准确、简便、灵敏,更适用于注射用阿洛西林钠的有关物质检测.

Objective To establish a suitable ultra-performance liquid chromatography for the determination of the related substances of azlocillion sodium for injection. The parts of related substances in azlocillion sodium for Injection were identified by LC-MS. Method The UPLC method was carried out using a ACQUITY UPLC BEH C18 column （2. 1 mm× 100mm, 1.7mm）; The column temperature was 40℃ and the detection wavelength was 210nm; mobile phase A was 10mmol/L ammonium formate solution （adjust pH to 6.5 with ammonium hydroxide）, mobile phase B was 8mmol ammonium formate solution （acetonitrile/water=200/50）; the flow rate was 0.43mL/min. Results Azlocillion sodium and its related substances could be well isolated. The method can detect more impurities than pharmacopoeia of China （2010）. The linear range of azlocillion was 0.3-90μg/mL（r2=0.9999）, The detection limit of azlocillion sodium was 0. 1μg/mL.The RSD of precision was 0.61%（n=6）. Conclusion The method is much higher chromatographic performance than existing national standard method. The method is accurate, simple and sensitive. It is more suitable for determination of the related substances of azlocillion sodium for injection.