Compendial Development Laboratory, United States Pharmacopeial Convention (USP), 12601 Twinbrook Parkway, Rockville, MD, 20852, USA.
Compendial Development Laboratory, United States Pharmacopeial Convention (USP), 12601 Twinbrook Parkway, Rockville, MD, 20852, USA.
J Pharm Biomed Anal. 2021 Feb 20;195:113858. doi: 10.1016/j.jpba.2020.113858. Epub 2020 Dec 31.
A rapid, sensitive, and accurate high-performance liquid chromatography (HPLC) method was developed and validated for the separation and analysis of organic impurities in erythromycin stearate tablets. The method separates Erythromycin, Erythromycin B, Erythromycin C and nine impurities (EP Impurity A, B, C, D, E, F, H, I and M). The chromatographic separation was achieved on a Waters XBridge C18 (100 mm × 4.6 mm, 3.5 μm) column. The mobile phase comprised of 0.4 % ammonium hydroxide in water and methanol delivered in a gradient mode. The compounds of interest were monitored at 215 nm. The stability-indicating capability of this method was evaluated by performing stress studies. Erythromycin was found to degrade significantly under acid, base, and oxidative stress conditions and it was only stable under thermal and photolytic degradation conditions. The degradation products were well resolved from the erythromycin peaks. In addition, the major degradants formed under stress conditions were characterized by ultra-high-performance liquid chromatography coupled with Single-Quadrupole Mass Spectrometer (UHPLC-QDa). The method was validated to fulfill International Conference on Harmonization (ICH) requirements and this validation included specificity, linearity, limit of detection (LOD), limit of quantification (LOQ), accuracy, precision, and robustness. The developed method could be incorporated into the USP monograph and applied for routine quality control analysis of erythromycin stearate tablets.
建立并验证了一种用于分离和分析硬脂酸红霉素片中有机杂质的快速、灵敏、准确的高效液相色谱（HPLC）方法。该方法可分离红霉素、红霉素 B、红霉素 C 和 9 种杂质（EP 杂质 A、B、C、D、E、F、H、I 和 M）。色谱分离在 Waters XBridge C18（100mm×4.6mm，3.5μm）柱上进行。流动相由水中 0.4%的氨和甲醇以梯度模式输送。感兴趣的化合物在 215nm 处监测。通过进行稳定性研究评估了该方法的稳定性指示能力。在酸、碱和氧化条件下，红霉素显著降解，仅在热和光降解条件下稳定。降解产物与红霉素峰很好地分离。此外，在应激条件下形成的主要降解产物通过超高效液相色谱与单四极杆质谱联用（UHPLC-QDa）进行了表征。该方法经过验证，符合国际协调会议（ICH）的要求，该验证包括专属性、线性、检测限（LOD）、定量限（LOQ）、准确度、精密度和耐用性。该方法可纳入 USP 专论，并应用于硬脂酸红霉素片的常规质量控制分析。
