亲水液体相互作用色谱法定量枸橼酸托法替尼及其相关物质的稳定性指示高效液相色谱法的开发与验证

IF 1.3 Q4 CHEMISTRY, ANALYTICAL
G. Sivaprasadu, Muralidhar Pamerla, Podilapu Atchutha Rao, Adapa Venkateswara Rao, Suresh Salakolusu, Harihara Padhy, Ravikumar Ganta
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引用次数: 0

摘要

针对枸橼酸托法替尼及其相关物质开发并验证了一种运行时间短的新型稳定性指示RPHPLC方法。该新型高效液相色谱法采用亲水相互作用液相色谱(HILIC)技术作为固定相,以磷酸盐缓冲液(pH 7.0)和乙腈(45:55, %v/v)为流动相,流速为0.5 mL/min,等度洗脱。通过 210 nm 波长的紫外检测器对分析物进行监测,柱温为 30°C,分析时间为 20 分钟。杂质-A、杂质-B 和托法替尼的精密度(%RSD)分别为 2.4%、0.8% 和 0.0%,符合规范要求。杂质的准确度从 86% 到 100% 不等,LOD 为 0.03%,LOQ 为 0.05%-0.06%。杂质与枸橼酸托法替尼的相关系数超过 0.999。室温下 24 小时的溶液稳定性得到确认。杂质的方法定量范围为LOQ~1.5%,枸橼酸托法替尼的方法定量范围为LOQ~150%。在酸和碱水解、氧化和水分解、热降解和光降解条件下对该方法的稳定性进行了评价。在这项工作中采用 HILIC 作为固定相证明是有效的,无需离子对试剂,缩短了分析时间,并确保了结果的一致性。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
Stability‐Indicating HPLC Method Development and Validation for the Quantification of Tofacitinib Citrate and Its Related Substances Using Hydrophilic Liquid Interaction Chromatography
A new stability‐indicating RPHPLC method with short run time has been developed and validated for tofacitinib citrate and its related substances. The novel HPLC method integrates hydrophilic interaction liquid chromatography (HILIC) technology as the stationary phase and employs a mobile phase composed of phosphate buffer (pH 7.0) and acetonitrile (45:55, %v/v) at a flow rate of 0.5 mL/min under isocratic elution. Analytes were monitored via a UV detector at 210 nm and with the column oven temperature at 30°C for a 20‐min analysis. Precision (%RSD) for Impurity‐A and Impurity‐B and tofacitinib met specifications at 2.4%, 0.8%, and 0.0%, respectively. Accuracy ranged from 86% to 100% for impurities, with LOD at 0.03% and LOQ at 0.05%–0.06%. Correlation coefficients exceeded 0.999 for impurities and tofacitinib citrate. Solution stability was confirmed for 24 h at room temperature. The method range was extended from LOQ to ∼1.5% for impurities and LOQ to ∼150% for tofacitinib citrate. The method's stability was evaluated under acid and base hydrolysis, oxidative and water hydrolysis, and thermal and photolytic degradation. Introducing HILIC as the stationary phase for this work proved effective, eliminating the need of ion pair reagents, reducing analysis time, and ensuring consistent results.
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来源期刊
SEPARATION SCIENCE PLUS
SEPARATION SCIENCE PLUS CHEMISTRY, ANALYTICAL-
CiteScore
1.90
自引率
9.10%
发文量
111
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