Izat Nihan, Kaplan Ozan, Çelebier Mustafa, Sahin Selma
Department of Pharmaceutical Technology, Hacettepe University Faculty of Pharmacy, Ankara 06800, Turkey.
Department of Analytical Chemistry, Hacettepe University Faculty of Pharmacy, Ankara 06100, Turkey.
ACS Omega. 2024 Apr 18;9(17):19250-19260. doi: 10.1021/acsomega.4c00109. eCollection 2024 Apr 30.
The isolated perfused rat liver (IPRL) model provides a mechanistic understanding of the organic-anion-transporting polypeptide (OATP/Oatp)-mediated pharmacokinetics in the preclinical evaluation, which often requires the use of control substrates (i.e., pitavastatin) and monitoring endogenous biomarkers (coproporphyrin I and III). This study aimed to develop and validate an LC-MS method allowing the simultaneous quantification of pitavastatin, coproporphyrin I (CPI), and coproporphyrin III (CPIII) in rat liver perfusion matrices (perfusate, liver homogenate, bile). The analysis was performed on a C18 column at 60 °C with 20 μL of sample injection. The mobile phases consisted of water with 0.1% formic acid and acetonitrile with 0.1% formic acid with a gradient flow of 0.5 mL/min. The assay was validated according to the ICH M10 Bioanalytical Method Validation Guideline (2022) for selectivity, calibration curve and range, matrix effect, carryover, accuracy, precision, and reinjection reproducibility. The method allowing the simultaneous quantification of pitavastatin, CPI, and CPIII was selective without having carryover and matrix effects. The linear calibration curves were obtained within various calibration ranges for three analytes in different matrices. Accuracy and precision values fulfilled the required limits. After 60 min perfusion with pitavastatin (1 μM), the cumulative amounts of pitavastatin in the liver and bile were 5.770 ± 1.504 and 0.852 ± 0.430 nmol/g liver, respectively. CPIII was a more dominant marker than CPI in both liver (0.028 ± 0.017 vs 0.013 ± 0.008 nmol/g liver) and bile (0.016 ± 0.011 vs 0.009 ± 0.007 nmol/g liver). The novel and validated bioanalytical method can be applied in further IPRL preparations investigating Oatp-mediated pharmacokinetics and DDIs.
离体灌注大鼠肝脏(IPRL)模型为临床前评估中有机阴离子转运多肽(OATP/Oatp)介导的药代动力学提供了机制上的理解,临床前评估通常需要使用对照底物(即匹伐他汀)并监测内源性生物标志物(粪卟啉I和III)。本研究旨在开发并验证一种液相色谱 - 质谱方法,用于同时定量大鼠肝脏灌注基质(灌注液、肝脏匀浆、胆汁)中的匹伐他汀、粪卟啉I(CPI)和粪卟啉III(CPIII)。分析在60℃的C18柱上进行,进样量为20μL。流动相由含0.1%甲酸的水和含0.1%甲酸的乙腈组成,梯度流速为0.5 mL/min。根据国际人用药品注册技术协调会(ICH)M10生物分析方法验证指南(2022)对该测定法进行选择性、校准曲线和范围、基质效应、残留、准确度、精密度和再进样重现性的验证。该同时定量匹伐他汀、CPI和CPIII的方法具有选择性,无残留和基质效应。在不同基质中,三种分析物在各种校准范围内均获得了线性校准曲线。准确度和精密度值符合要求的限度。用匹伐他汀(1μM)灌注60分钟后,肝脏和胆汁中匹伐他汀的累积量分别为5.770±1.504和0.852±0.430 nmol/g肝脏。在肝脏(0.028±0.017对0.013±0.008 nmol/g肝脏)和胆汁(0.016±0.011对0.009±0.007 nmol/g肝脏)中,CPIII都是比CPI更主要的标志物。这种新的且经过验证的生物分析方法可应用于进一步研究Oatp介导的药代动力学和药物相互作用的IPRL制剂中。