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首页> 外文期刊>Journal of mass spectrometry: JMS >Stepwise optimization approach for improving LC-MS/MS analysis of zwitterionic antiepileptic drugs with implementation of experimental design
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Stepwise optimization approach for improving LC-MS/MS analysis of zwitterionic antiepileptic drugs with implementation of experimental design

机译：通过实验设计改进逐步改善两性离子抗癫痫药LC-MS / MS分析的方法

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摘要

In this article, a step-by-step optimization procedure for improving analyte response with implementation of experimental design is described. Zwitterionic antiepileptics, namely vigabatrin, pregabalin and gabapentin, were chosen as model compounds to undergo chloroformate-mediated derivatization followed by liquid chromatography coupled with tandem mass spectrometry (LC-MS/MS) analysis. Application of a planned stepwise optimization procedure allowed responses of analytes, expressed as areas and signal-to-noise ratios, to be improved, enabling achievement of lower limit of detection values. Results from the current study demonstrate that optimization of parameters such as scan time, geometry of ion source, sheath and auxiliary gas pressure, capillary temperature, collision pressure and mobile phase composition can have a positive impact on sensitivity of LC-MS/MS methods. Optimization of LC and MS parameters led to a total increment of 53.9%, 83.3% and 95.7% in areas of derivatized vigabatrin, pregabalin and gabapentin, respectively, while for signal-to-noise values, an improvement of 140.0%, 93.6% and 124.0% was achieved, compared to autotune settings. After defining the final optimal conditions, a time-segmented method was validated for the determination of mentioned drugs in plasma. The method proved to be accurate and precise with excellent linearity for the tested concentration range (40.0 ng ml~(-1)-10.0×10~3 ng ml~(-1)).
机译：在本文中，描述了通过实施实验设计来改善分析物响应的分步优化程序。选择两性离子抗癫痫药，即vigabatrin，pregabalin和gabapentin作为模型化合物，进行氯甲酸酯介导的衍生化，然后进行液相色谱和串联质谱（LC-MS / MS）分析。计划的逐步优化程序的应用允许改善分析物的响应（表示为面积和信噪比），从而实现检测值的下限。当前研究的结果表明，优化参数（例如扫描时间，离子源的几何形状，鞘和辅助气体压力，毛细管温度，碰撞压力和流动相组成）可以对LC-MS / MS方法的灵敏度产生积极影响。 LC和MS参数的优化导致衍生化的维加巴特林，普瑞巴林和加巴喷丁的区域分别增加了53.9％，83.3％和95.7％，而信噪比分别提高了140.0％，93.6％和59.7％。与自动调谐设置相比，达到了124.0％。确定最终的最佳条件后，验证了一种时间分段方法，用于测定血浆中的上述药物。在所测浓度范围（40.0 ng ml〜（-1）-10.0×10〜3 ng ml〜（-1））下，该方法被证明是准确和精确的，并具有出色的线性。

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