HPLC法测定甲磺酸奥希替尼的含量
Determination of osimertinib mesylate by HPLC
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摘要: 为了建立一种检测甲磺酸奥希替尼含量的HPLC法，使用Agilent ZORBAX Eclipse Plus C18色谱柱(4.6 mm×250 mm，5 μm)，流动相为甲醇-磷酸二氢钠缓冲液(pH 3.0)(50∶50)，检测波长210 nm，柱温35 ℃，流速1.0 mL/min进行检测。甲磺酸奥希替尼浓度在分析物正常浓度的50%~150%(0.201 1~0.603 2 mg/mL)范围内与峰面积呈良好线性关系(r=0.999 9)，最低检测限为0.08 μg/mL，定量限为0.32 μg/mL。3批样品的含量(%)分别为100.1、99.5和99.7。在所建立的色谱条件下，甲磺酸奥希替尼与各有关物质分离良好，包括部分工艺杂质及降解杂质。结果表明，所建立的方法专属、准确、简单、耐用，可用于奥希替尼原料的含量测定。Abstract: To establish an HPLC method to determine osimertinib mesylate, Agilent ZORBAX Eclipse Plus C18 column(4. 6 mm × 250 mm, 5 μm)was used with a mobile phase consisting of methanol-buffer solution(20 mmol/L NaH2PO4, pH 3. 0 adjusted with 85% H3PO4)(50 ∶50)at the flow rate of 1. 0 mL/min. The detection wavelength was 210 nm, and the column temperature was kept at 35 ℃. The calibration curve was liner over the range from 50% to 150% of determination concentration(0. 201 1- 0. 603 2 mg/mL, r=0. 999 9). The limit of quantitation(LOQ)and limit of detection(LOD)were 0. 32 μg/mL and 0. 08 μg/mL, respectively. The contents of osimertinib mesylate in samples were 100. 1%, 99. 5% and 99. 7%. Good chromatographic separation of osimertinib mesylate and its related substances, including synthetic impurities and degradation products, were obtained. The established HPLC method is specific, accurate, simple and durable, and could be used for the determination of osimertinib mesylate.
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Keywords:
- osimertinib mesylate /
- HPLC /
- determination /
- related substances
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