Development and validation of a reversed‐phase high‐performance liquid chromatography–ultraviolet method for abemaciclib‐related substance detection in bulk drugs. Issue 22 (20th September 2022)

• Record Type: Journal Article
• Authors: Ni, Ronghua; Du, Xiao; Huang, Rongrong; Wu, Wenyi; Xu, Jingqiu; Ma, Xiaofei; Cai, Liangliang
• Is Part Of: Journal of separation science. Volume 45:Issue 22(2022)
• Page Start: 4070
• Page End: 4078
• Publication Date: 2022-09-20
• Subjects: abemaciclib -- impurity detection -- liquid chromatography -- method development -- method validation; Separation (Technology) -- Periodicals; Chromatographic analysis -- Periodicals; 543.089
• DOI: 10.1002/jssc.202200551
• Languages: English
• ISSNs: 1615-9306

Abstract

Abstract : Abemaciclib is an effective selective cyclin‐dependent kinases 4 and 6 inhibitors for cancer therapy. The abemaciclib‐related substances influence its efficacy and safety, and are important in process preparation studies and quality control. Thus, a reversed‐phase high‐performance liquid chromatography method was developed and validated for the detection of related substances in its bulk drug. The separation of abemaciclib and related substances was performed on a Phenomenon Gemini C18 column (4.6 × 250 mm, 5 μm) with a flow rate of 1.0 ml/min. The ultraviolet detection wavelength was 280 nm. Mobile phase A was composed of a mixed solution of aqueous solution and acetonitrile (9:1, v/v). The aqueous solution (pH 2.5) contained 0.025‐mM potassium dihydrogen phosphate solution and 0.4% triethylamine. Mobile phase B was composed of acetonitrile. This novel method exhibits good system suitability, specificity, precision, stability, linearity (0.1–20 μg/ml), repeatability, and durability. Among abemaciclib and related substances, the lowest limit of detection and quantitation were 0.02 and 0.06 μg/ml, respectively, for abemaciclib. The recovery rates for related substances were above 95%. In addition, a novel degradation product was found during the process. In summary, a reliable reversed‐phase high‐performance liquid chromatography method was developed for abemaciclib‐related substance detection in bulk drugs.