高效液相色谱法同时测定细芬烯酮和卡格列净在代谢稳定性研究中的应用。

IF 1.8 4区医学 Q3 BIOCHEMICAL RESEARCH METHODS

Bioanalysis Pub Date : 2025-09-29 DOI:10.1080/17576180.2025.2565142

Shivam Rathaur, Parag Varshney, Sachin Vishwakarma, Debalina Maity, Sharib R Khan, Jiaur R Gayen

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引用次数: 0

摘要

目的：建立一种快速、灵敏、可靠的高效液相色谱法同时测定芬内烯酮（FNR）和卡格列净（CFZ）的含量。方法：采用流动相乙腈（ACN）：水（51:49），流速为0.75 ml/min， C18色谱柱Phenomenex Luna （250 mm, 4.6 mm, 5µm）。FNR和CFZ的保留时间分别为6.33和8.26 min，分析运行时间为10.0 min，用PDA检测器检测，λ最大波长分别为249 nm和290 nm。FNR和CFZ在0.05 ~ 10µg/ml范围内呈线性关系，R2分别为0.998和0.999。FNR和CFZ的检出限分别为0.53和0.36 μg/ml，定量限分别为1.62和1.10 μg/ml。通过特异性、线性度、准确度、精密度、定量限、鲁棒性和稳定性对方法进行验证。结论：根据国际统一委员会（ICH）指南，验证研究证实该优化方法具有特异性、简单性、高灵敏度、可靠、稳健和可重复性。该方法已成功应用于人、猴、狗、兔、大鼠和小鼠混合微粒体的体外代谢稳定性研究。

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Simultaneous estimation of finerenone and canagliflozin using HPLC: application in metabolic stability studies.

Aim: A robust, sensitive, and reliable method was developed and validated on HPLC for the simultaneous estimation of Finerenone (FNR) and Canagliflozin (CFZ).

Method: The resolution was performed by using mobile-phase acetonitrile (ACN): Water (51:49) at a flow rate of 0.75 ml/min with the C18 analytical column Phenomenex Luna (250 mm, 4.6 mm, 5 µm). FNR and CFZ were estimated at a retention time of 6.33 and 8.26 min with 10.0 min analysis run time and detected by PDA detector at a λ_max 249 and 290 nm, respectively. The calibration curve was linear over the concentration range of 0.05-10 µg/ml with R² 0.998 and 0.999 for FNR and CFZ, respectively. For FNR and CFZ, the limit of detection (LOD) was 0.53 and 0.36 μg/ml & limit of quantitation (LOQ) was 1.62 and 1.10 μg/ml, respectively. The method was validated using specificity, linearity, accuracy, precision, LOD, LOQ, robustness, and stability.

Conclusion: According to the International Council for Harmonisation (ICH) guideline, the validation studies confirmed that the optimization method is specific, simple, highly sensitive, reliable, robust, and reproducible. The developed method was successfully applied for simultaneous estimation with applications in in-vitro metabolic stability studies of pooled microsomes of humans, monkeys, dogs, rabbits, rats and mice.

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来源期刊

Bioanalysis BIOCHEMICAL RESEARCH METHODS-CHEMISTRY, ANALYTICAL

CiteScore

3.30

自引率

16.70%

发文量

审稿时长

2 months

期刊介绍： Reliable data obtained from selective, sensitive and reproducible analysis of xenobiotics and biotics in biological samples is a fundamental and crucial part of every successful drug development program. The same principles can also apply to many other areas of research such as forensic science, toxicology and sports doping testing. The bioanalytical field incorporates sophisticated techniques linking sample preparation and advanced separations with MS and NMR detection systems, automation and robotics. Standards set by regulatory bodies regarding method development and validation increasingly define the boundaries between speed and quality. Bioanalysis is a progressive discipline for which the future holds many exciting opportunities to further reduce sample volumes, analysis cost and environmental impact, as well as to improve sensitivity, specificity, accuracy, efficiency, assay throughput, data quality, data handling and processing. The journal Bioanalysis focuses on the techniques and methods used for the detection or quantitative study of analytes in human or animal biological samples. Bioanalysis encourages the submission of articles describing forward-looking applications, including biosensors, microfluidics, miniaturized analytical devices, and new hyphenated and multi-dimensional techniques. Bioanalysis delivers essential information in concise, at-a-glance article formats. Key advances in the field are reported and analyzed by international experts, providing an authoritative but accessible forum for the modern bioanalyst.