采用质量源于设计方法,系统优化反相超高效液相色谱法定量检测散装药物和药物制剂中的尼洛替尼及其相关物质

IF 1.3 Q4 CHEMISTRY, ANALYTICAL SEPARATION SCIENCE PLUS Pub Date : 2024-02-07 DOI:10.1002/sscp.202300185
Shishir Kumar Prasad, Divekar Kalpana
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引用次数: 0

摘要

建立了一种灵敏的超高效液相色谱(UHPLC)方法,用于定量检测尼洛替尼胶囊剂中的痕量尼洛替尼及其相关物质(RSs)。采用ACQUITY UHPLC BEH Phenyl色谱柱(2.1 × 100 mm, 1.7 μm),流速为0.6 mL/min,通过实验设计优化了方法的关键参数。由水相和有机相组成的等度流动相在 8 分钟内实现了高效色谱分离,波长 261 nm。尼洛替尼的平均保留时间为 6.1339 分钟,RSs 的平均保留时间为 2.10 至 6.91 分钟,所有峰的分辨率均超过 2。该方法具有稳健性,可分离已知杂质和降解产物。线性范围为尼洛替尼 0.02-80 ppm,杂质 0.015-0.12 ppm。尼洛替尼的检测限和定量限(LOQ)分别为 0.01 和 0.02 μg/mL,各杂质的检测限和定量限(LOQ)分别为 0.01 和 0.015 μg/mL。在 LOQ、100% 和 150% 规格限下进行的回收率研究得出的回收率为 92.27% 至 102.45%。精密度结果显示相对标准偏差较低,尼洛替尼的相对标准偏差低于 2%,杂质的相对标准偏差低于 8%。该方法适用于药物制剂的定量分析。
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Systematic optimization of reverse phase ultra‐high‐performance liquid chromatography method for quantification of nilotinib and its related substances in bulk drug and pharmaceutical formulation using quality by design approach
A sensitive ultra‐high‐performance liquid chromatography (UHPLC) method was developed for the quantification of trace levels of nilotinib and its related substances (RSs) in the nilotinib capsule dosage form. Critical method parameters were optimized using the design of experiments, employing the ACQUITY UHPLC BEH Phenyl column (2.1 × 100 mm, 1.7 μm) at a constant flow rate of 0.6 mL/min. The isocratic mobile phase, consisting of aqueous and organic phases, achieved efficient chromatographic separation within 8 min at 261 nm. The mean retention time for nilotinib was 6.1339, and for RSs, it ranged from 2.10 to 6.91 min, with a resolution exceeding 2 for all peaks. The method demonstrated robustness, separating known impurities and degradation products. The linearity was assessed over a concentration range of 0.02–80 ppm for nilotinib and 0.015–0.12 ppm for impurities. The limit of detection and limit of quantitation (LOQ) for nilotinib were 0.01 and 0.02 μg/mL, respectively, and 0.01 and 0.015 μg/mL for individual impurities. Recovery studies at LOQ, 100%, and 150% of the specification limit yielded percent recoveries ranging from 92.27% to 102.45%. Precision results showed low relative standard deviations, below 2% for nilotinib and below 8% for impurities. This method is deemed suitable for pharmaceutical formulation quantification.
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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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