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Low-Temperature Plasma Probe Mass Spectrometry for Analytes Separated on Thin-Layer Chromatography Plates: Direct vs Laser Assisted Desorption.
Journal of the American Society for Mass Spectrometry ( IF 3.1 ) Pub Date : 2020-08-18 , DOI: 10.1021/jasms.0c00246
Xiaoxia Gong 1 , Dong Zhang 1 , Inah B Embile 1 , Yue She 1 , Songyue Shi 1 , Gerardo Gamez 1
Affiliation  

Thin-layer chromatography (TLC) is a widespread technique because it allows fast, simple, and inexpensive analyte separations. In addition, direct analysis of the compounds separated on TLC plates via mass spectrometry (MS) has been shown to provide high sensitivity and selectivity while avoiding time-consuming sample extraction protocols. Here, direct desorption low-temperature plasma-mass spectrometry (LTP-MS) as well as diode laser assisted desorption (LD) LTP-MS are studied for direct spatially resolved analysis of compounds from TLC plates. Qualitative and quantitative characterization of amino acids, pharmaceuticals, and structural isomers were performed. The nature of the TLC plate stationary phase was found to have a significant influence, together with the analyte's characteristics, on the desorption efficiency. Tandem MS is shown to greatly improve the limits of detection (LODs). Direct desorption LTP-MS, without external thermal assisted desorption, demonstrates its best performance with cellulose TLC plates (LODs, 0.01 ng/mm2 to 2.55 ng/mm2) and restricted performance with normal-phase (NP) TLC plates (several analytes without observable signal). LD LTP-MS, with systematic optimization of irradiance and focal point diameter, is shown to overcome the direct-desorption limitations and reach significantly improved LODs with NP TLC plates (up to ×1000 better). In addition, a wide-ranging characterization of amino acid analytical figures of merit with LD LTP-MS shows that LODs from 84 pg/mm2 down to 0.3 pg/mm2 are achieved on NP TLC plates.

中文翻译:

薄层色谱板上分离的分析物的低温等离子体探针质谱:直接与激光辅助解吸。

薄层色谱(TLC)是一种广泛使用的技术,因为它可以快速,简单且廉价地分离分析物。此外,已显示通过质谱(MS)对TLC板上分离的化合物进行直接分析可提供高灵敏度和选择性,同时避免了费时的样品提取方案。在这里,研究了直接解吸低温等离子体质谱(LTP-MS)以及二极管激光辅助解吸(LD)LTP-MS,用于对TLC板中的化合物进行直接空间分辨分析。进行了氨基酸,药物和结构异构体的定性和定量表征。发现TLC板固定相的性质以及分析物的特性对解吸效率具有重要影响。串联质谱显示出可以大大提高检测限(LOD)。直接解吸LTP-MS无需外部热辅助解吸,证明了其在纤维素TLC板(LOD,0.01 ng / mm2至2.55 ng / mm2)上的最佳性能,而在正相(NP)TLC板上的性能有限(几种分析物均未观察到信号)。LD LTP-MS通过系统优化辐照度和焦点直径,克服了直接解吸的局限性,并使用NP TLC板达到了明显改善的LOD(最高可达1000倍)。此外,使用LD LTP-MS进行的氨基酸分析品质因数的广泛表征表明,在NP TLC板上可实现从84 pg / mm2降至0.3 pg / mm2的LOD。展示了其在纤维素TLC板(LOD,0.01 ng / mm2至2.55 ng / mm2)上的最佳性能,以及在正相(NP)TLC板(几种无可观察信号的分析物)下的最佳性能。LD LTP-MS通过系统优化辐照度和焦点直径,克服了直接解吸的局限性,并使用NP TLC板达到了明显改善的LOD(最高可达1000倍)。此外,使用LD LTP-MS进行的氨基酸分析品质因数的广泛表征表明,在NP TLC板上可实现从84 pg / mm2降至0.3 pg / mm2的LOD。展示了其在纤维素TLC板(LOD,0.01 ng / mm2至2.55 ng / mm2)上的最佳性能,以及在正相(NP)TLC板(几种无可观察信号的分析物)下的最佳性能。LD LTP-MS通过系统优化辐照度和焦点直径,克服了直接解吸的局限性,并使用NP TLC板达到了明显改善的LOD(最高可达1000倍)。此外,使用LD LTP-MS进行的氨基酸分析品质因数的广泛表征显示,在NP TLC板上可实现从84 pg / mm2降至0.3 pg / mm2的LOD。通过对辐照度和焦点直径进行系统优化,可以克服直接解吸的局限性,并使用NP TLC板达到显着改善的LOD(最高可达1000倍)。此外,使用LD LTP-MS进行的氨基酸分析品质因数的广泛表征显示,在NP TLC板上可实现从84 pg / mm2降至0.3 pg / mm2的LOD。通过对辐照度和焦点直径进行系统优化,可以克服直接解吸的局限性,并使用NP TLC板达到显着改善的LOD(最高可达1000倍)。此外,使用LD LTP-MS进行的氨基酸分析品质因数的广泛表征表明,在NP TLC板上可实现从84 pg / mm2降至0.3 pg / mm2的LOD。
更新日期:2020-08-18
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