一种简单的核壳柱超高效液相色谱-质谱联用法测定人血浆中依西美坦的临床应用。

Takuho Ishii, Nana Nojiri, Yuji Mano
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引用次数: 0

摘要

依西美坦是芳香化酶抑制剂之一,通过降低雌激素水平来治疗乳腺癌。为确定依西美坦的最佳剂量,建立了依西美坦的超高效液相色谱串联质谱分析方法。用乙腈/甲醇(1/1,v/v)简单蛋白沉淀法从人血浆样品(100 μL)中提取依西美坦。在依西美坦洗脱附近观察到的干扰峰使我们使用核壳柱而不是全孔柱具有更高的选择性。提取液在CORTECS UPLC C18上进行层析,梯度洗脱,流速0.25 mL/min,在所选反应监测中检测。根据生物分析指南使用质量控制样品评估验证参数。依西美坦在人血浆中的定量范围为0.5 ~ 50 ng/mL,提取回收率高,基质效应小。溶血或高脂血症血浆不影响依西美坦试验。依西美坦在-15°C或更低温度下在人血浆中稳定392天。开发的分析是稳健的,并成功地应用于定量人血浆中的依西美坦浓度,以支持临床试验。
本文章由计算机程序翻译,如有差异,请以英文原文为准。
A simple UPLC-MS/MS assay with a core-shell column for the determination of exemestane in human plasma for clinical application.

Exemestane is one of the aromatase inhibitors and has been used to treat breast cancer by lowering estrogen levels. Accurate quantification of exemestane is important to set an optimal dose, and thus a simple assay for exemestane is developed by ultra-performance liquid chromatography with tandem mass spectrometer. Exemestane was extracted from human plasma samples (100 μL) by simple protein precipitation with acetonitrile/methanol (1/1, v/v). Interference peaks observed close to the elution of exemestane led us to use a core shell column for higher selectivity instead of totally porous columns. The extracts were chromatographed on CORTECS UPLC C18, under a gradient elution at a flow rate of 0.25 mL/min and detected in the selected reaction monitoring. Validation parameters were assessed in accordance with the bioanalytical guidelines using quality control samples. Exemestane in human plasma was quantifiable from 0.5 to 50 ng/mL with high extraction recovery and minimal matrix effects. Hemolyzed or hyperlipemic plasma did not impact the exemestane assay. Exemestane was stable in human plasma for 392 days at -15°C or below. The developed assay was robust and successfully applied to quantifying exemestane concentrations in human plasma to support a clinical trial.

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