Analytical and Bioanalytical Chemistry ( IF 3.8 ) Pub Date : 2022-08-17 , DOI: 10.1007/s00216-022-04276-0 Maria Fernanda Cifuentes Girard 1 , Patrick Knight 2 , Roger Giles 2 , Gérard Hopfgartner 1
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The effect of LC mobile phase composition and flow rate (2–50 µL/min) on mobility behavior in vacuum differential mobility spectrometry (vDMS) was investigated for electrosprayed isobaric antidepressant drugs (AD); amitriptyline, maprotiline, venlafaxine; and structurally related antidepressants nortriptyline, imipramine, and desipramine. While at 2 µL/min, no difference in compensation voltage was observed with methanol and acetonitrile, at 50 µL/min, acetonitrile used for LC elution of analytes enabled the selectivity of the mobility separation to be improved. An accurate and sensitive method could be developed for the quantification of six AD drugs in human plasma using trap/elute micro-LC setup hyphenated to vDMS with mass spectrometric detection in the selected ion monitoring mode. The assay was found to be linear over three orders of magnitude, and the limit of quantification was of 25 ng/mL for all analytes. The LC-vDMS-SIM/MS method was compared to a LC-MRM/MS method, and in both cases, inter-assay precisions were lower than 12.5 and accuracies were in the range 91.5–110%, but with a four times reduced analysis time (2 min) for the LC-vDMS-SIM/MS method. This work illustrates that with vDMS, the LC mobile phase composition can be used to tune the ion mobility separation and to improve assay selectivity without additional hardware.
Graphical abstract
中文翻译：
液相色谱流动相在真空差示迁移谱-质谱法中对人血浆中抗抑郁药物选择性分析的影响
研究了电喷雾等压抗抑郁药物 (AD) 的 LC 流动相组成和流速 (2–50 µL/min) 对真空差示迁移谱 (vDMS) 迁移行为的影响；阿米替林、马普替林、文拉法辛；和结构相关的抗抑郁药去甲替林、丙咪嗪和地昔帕明。虽然在 2 µL/min 时，甲醇和乙腈没有观察到补偿电压的差异，但在 50 µL/min 时，用于 LC 洗脱分析物的乙腈能够提高迁移率分离的选择性。可以开发一种准确且灵敏的方法，用于定量人血浆中的六种 AD 药物，该方法使用与 vDMS 联用的捕获/洗脱微型 LC 设置，并在选定的离子监测模式下进行质谱检测。发现该测定在三个数量级上呈线性，所有分析物的定量限为 25 ng/mL。将 LC-vDMS-SIM/MS 方法与 LC-MRM/MS 方法进行比较，在这两种情况下，测定间精密度均低于 12.5，准确度在 91.5-110% 范围内，但降低了四倍LC-vDMS-SIM/MS 方法的分析时间（2 分钟）。这项工作表明，使用 vDMS，LC 流动相组成可用于调整离子淌度分离并提高分析选择性，而无需额外的硬件。但 LC-vDMS-SIM/MS 方法的分析时间（2 分钟）缩短了四倍。这项工作表明，使用 vDMS，LC 流动相组成可用于调整离子淌度分离并提高分析选择性，而无需额外的硬件。但 LC-vDMS-SIM/MS 方法的分析时间（2 分钟）缩短了四倍。这项工作表明，使用 vDMS，LC 流动相组成可用于调整离子淌度分离并提高分析选择性，而无需额外的硬件。
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