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首页> 外文期刊>Journal of chromatography, B. Analytical technologies in the biomedical and life sciences >Screening of cardiovascular agents in plasma with LC-MS/MS: A valuable tool for objective drug adherence assessment
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Screening of cardiovascular agents in plasma with LC-MS/MS: A valuable tool for objective drug adherence assessment

机译：用LC-MS / MS筛选血浆中的心血管剂：目标药物依从性评估的宝贵工具

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摘要

Adherence to cardiovascular preventive agents is important to prevent short and long term cardiovascular events. Recently, qualitatively compound screening using liquid chromatography-tandem mass spectrometry (LC-MS/MS) has gained interest for drug adherence assessment in patients at high risk of cardiovascular events. Therefore, we developed and tested an assay including 52 compounds and metabolites, covering over 95% of the antihypertensive and antithrombotic agents available worldwide. Trichloroacetic acid was used as simple and fast method for protein precipitation. The assay was validated for lower limit of quantification (LLOQ), linearity, stability for freeze/thaw, room temperature, autosampler and matrix effects. The LLOQ for each compound was targeted under the population trough concentration (PTC) as reported in literature to assure high sensitivity for adherence detection. This was accomplished for 50 of 52 compounds with a LLOQ equal or lower compared to the PTC. Linearity was confirmed for all compounds (r(2) > 0.995), except for acetylsalicylic acid (r(2) = 0.991). For room temperature stability, 12 compounds showed degradation over 20% after 20 h. 3 compounds suffer from matrix effect with recoveries < 50%. After analytical validation, blood samples from 91 patients with difficult-to-treat hypertension were analyzed. Patients were unaware of adherence assessment. Adherence varied largely per agent and per concentration ratio (CR) (ratio of the detected concentration with LC-MS/MS and the PTC) cut-off value. Additionally, stratification by adherence group showed that the percentage of patients classified as non-adherent increased from 6.6% for qualitative analysis (pos/neg) to 19.8% for a CR cut-off of 0.5. The data imply that using the CR cut off values has a significant and relevant effect on patient adherence classification.
机译：坚持心血管预防剂对预防短期和长期心血管事件非常重要。最近，使用液相色谱 - 串联质谱（LC-MS / MS）的定性化合物筛选对心血管事件的高风险患者的药物依从性评估感兴趣。因此，我们开发并测试了包括52种化合物和代谢物的测定，占据全球可用的95％的抗高血压和抗血栓形成剂。使用三氯乙酸作为蛋白质沉淀的简单和快速方法。测定验证用于较低定量限制（LLOQ），线性度，冻融稳定性，室温，自动进样器和矩阵效应的较低限度。每种化合物的LLOQ靶向文献中报道的人口槽浓度（PTC），以确保粘附检测的高灵敏度。与PTC相比，将其为52个化合物中的50个，其中LLOQ等于或更低。除乙酰胱氨酸外（R（2）= 0.991）外，还确认了所有化合物（R（2）> 0.995）的线性。对于室温稳定，12种化合物在20小时后显示出超过20％的降解。 3化合物患有基质效应，回收率<50％。分析验证后，分析了91例难以治疗的高血压患者的血液样本。患者没有意识到依从性评估。粘附性主要是每种药剂和每浓度比（Cr）（检测到的浓度与LC-MS / MS和PTC的比率）截止值。此外，依从项的分层表明，归类为非抗粘附的患者的百分比从6.6％增加到定性分析（POS / NEN），为0.5的CR切断的CR截止值为19.8％。数据意味着使用CR切断值对患者依从性分类具有重要且相关的影响。

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