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建立并验证一种 LC-MS/MS 检测方法，用于定量检测小鼠血浆中的 MO-OH-Nap 萘醍酮：应用于体外和体内药代动力学研究。

Development and Validation of an LC-MS/MS Assay for the Quantitation of MO-OH-Nap Tropolone in Mouse Plasma: Application to In Vitro and In Vivo Pharmacokinetic Studies.

机构信息

Department of Pharmacy Practice and Science, College of Pharmacy, University of Nebraska Medical Center, Omaha, NE 68198, USA.

Department of Internal Medicine, University of Nebraska Medical Center, Omaha, NE 68198, USA.

出版信息

Molecules. 2024 Sep 18;29(18):4424. doi: 10.3390/molecules29184424.

DOI:10.3390/molecules29184424
PMID:39339419
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC11434026/
Abstract

A rapid, selective, and sensitive liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) method was developed and validated for the quantitation of MO-OH-Nap tropolone (MO-OH-Nap) in mouse plasma. MO-OH-Nap is an α-substituted tropolone with anti-proliferative properties in various cancer cell lines. Detection and separation of analytes was achieved on an ACE Excel C18 (1.7 µm, 100 × 2.1 mm, MAC-MOD Analytical, Chadds Ford, PA, USA) column with mobile phase consisting of 0.05% trifluoroacetic acid in water (mobile phase A) and 0.05% trifluoroacetic acid in acetonitrile (mobile phase B), with an isocratic elution of 15:85% (A:B) at a total flow rate of 0.25 mL/min. The LC-MS/MS system was operated at unit resolution in multiple reaction monitoring (MRM) mode, using precursor ion > product ion combination of 249.10 > 202.15 / for MO-OH-Nap and 305.10 > 215.05 / for the internal standard (IS), BA-SM-OM. The MS/MS response was linear over a concentration range of 1 to 500 ng/mL with a correlation coefficient (r) of ≥0.987. The within- and between-batch precision (%RSD) and accuracy (%Bias) were within acceptable limits. The validated method was successfully applied to determine MO-OH-Nap metabolic stability, plasma protein binding, and bio-distribution studies of MO-OH-Nap in CD-1 mice.

摘要

建立并验证了一种快速、选择性和灵敏的液相色谱-串联质谱（LC-MS/MS）方法，用于定量检测小鼠血浆中的 MO-OH-Nap 硝酮（MO-OH-Nap）。MO-OH-Nap 是一种α取代的硝酮，在多种癌细胞系中具有抗增殖特性。分析物的检测和分离是在 ACE Excel C18（1.7 µm，100 × 2.1 mm，MAC-MOD Analytical，Chadds Ford，PA，USA）柱上实现的，流动相由 0.05%三氟乙酸水溶液（流动相 A）和 0.05%三氟乙酸乙腈溶液（流动相 B）组成，采用等度洗脱，总流速为 0.25 mL/min，洗脱条件为 15:85%（A:B）。LC-MS/MS 系统在多重反应监测（MRM）模式下以单位分辨率运行，使用前体离子>产物离子组合 249.10 > 202.15 /用于 MO-OH-Nap，以及 305.10 > 215.05 /用于内标（IS）BA-SM-OM。MS/MS 响应在 1 至 500 ng/mL 浓度范围内呈线性，相关系数（r）≥0.987。日内和日间精密度（%RSD）和准确度（%偏差）均在可接受范围内。该验证方法成功应用于 CD-1 小鼠中 MO-OH-Nap 代谢稳定性、血浆蛋白结合和生物分布研究。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/d2819b4b5c5f/molecules-29-04424-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/45714cb72b8d/molecules-29-04424-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/a8037efc0e53/molecules-29-04424-g002a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/877fbc1b72e4/molecules-29-04424-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/5d54e4cf31e6/molecules-29-04424-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/e0aa46b54a97/molecules-29-04424-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/80420e1d299d/molecules-29-04424-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/d2819b4b5c5f/molecules-29-04424-g007.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/45714cb72b8d/molecules-29-04424-g001.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/a8037efc0e53/molecules-29-04424-g002a.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/877fbc1b72e4/molecules-29-04424-g003.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/5d54e4cf31e6/molecules-29-04424-g004.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/e0aa46b54a97/molecules-29-04424-g005.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/80420e1d299d/molecules-29-04424-g006.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/5a73/11434026/d2819b4b5c5f/molecules-29-04424-g007.jpg

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