Liquid Extraction Surface Analysis (LESA): A New Mass Spectrometry‐Based Technique for Ambient Surface Profiling

Eikel, Daniel; Henion, Jack D.

doi:10.1002/9781118516157.ch8

Mass Spectrometry for Drug Discovery and Drug Development 2013

DOI: 10.1002/9781118516157.ch8

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Liquid Extraction Surface Analysis (LESA): A New Mass Spectrometry‐Based Technique for Ambient Surface Profiling

Daniel Eikel

Jack D. Henion

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Cited by 3 publications

(5 citation statements)

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“…For instance, the development and subsequent application of slug-flow liquid–liquid microextraction inside a nano-ESI emitter for extraction of prohibited substances from different biofluids was shown to achieve acceptable limits of detection and preconcentration factors . In the solid–liquid microextraction area, several technologies for direct coupling, such as liquid extraction surface analysis (LESA), , open port sample interface (OPSI), − and the capillary gap sampler, have been reported. As one of their highlights, the above techniques are well-known for their superior speed of analysis, enabling times of analysis per sample of just a few seconds. , Although these technologies extract using the same concept, extraction time in OPSI and the capillary gap sampler cannot be optimized due to the dynamic nature of these technologies, which operate via a constant flow of solvent toward the mass spectrometer.…”

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confidence: 99%

Direct Coupling of Dispersive Extractions with Magnetic Particles to Mass Spectrometry via Microfluidic Open Interface

et al. 2019

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Microextraction coupled to MS has great potential in analytical chemistry laboratories operating in a variety of fields. Indeed, microextraction methods directly coupled to MS can be of large value given that they can provide not only analyte extraction and enrichment, but also effective sample cleanup. In recent years, the practicality in handling, high active surface area, versatility, and environmentally friendly features of magnetic dispersive microextraction technologies have contributed to an explosion in the number of methods and technologies reported in the literature for a wide range of applications. However, to the best of our knowledge, no technology to date has been capable of efficiently merging these two rising concepts in a simple and integrated analytical workflow. In this context, the microfluidic open interface is presented for the direct coupling of dispersive magnetic extraction to mass spectrometry. This technology operates under the concept of a flow-isolated desorption volume, which generates a stagnant droplet open to ambient while continuously feeding with solvent the ionization source by means of the self-aspiration process intrinsic of the ESI interface. To improve the efficiency of the final analytical workflow, a novel dispersive magnetic micro-and nanoparticle extraction protocol for biofluid droplets was developed. The final methodology entailed the dispersion of a small amount of magnetic particles (20-70 µg) in a droplet of biofluid (≤ 40 µL) for extraction, followed by a particle collection step using a home-made 3D-printed holder containing an embedded rare-earth magnet. In the final step, the holder is set on top of the MOI for desorption in the isolated droplet. By switching the valve, the desorbed analytes are transferred to the ESI source in less than 5 sec. As proof of concept, the completely new setup was applied to the determination of prohibited substances from PBS and human urine using Fe2O3 magnetic nanoparticles (50 nm) functionalized with C18. The LOQs obtained were in the low-ppb range in all cases, and acceptable precision (≤20%) and accuracy (80-120%) were attained. Also, taking advantage of the fast extraction kinetics provided by the radial diffusion associated with small particles, the methodology was employed for the selective extraction of phosphopeptides from 40 µL of tryptic β-casein digest using 70 µg of magnetic Ti-IMAC microparticles. To conclude, the technology and methodology herein presented provided excellent capabilities comparable to other SPME-MS approaches while dramatically minimizing the amount of sample and sorbent required per analysis, as well as affording significantly fast extraction times due to the enhanced kinetics of extraction.

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confidence: 99%

Direct Coupling of Dispersive Extractions with Magnetic Particles to Mass Spectrometry via Microfluidic Open Interface

et al. 2019

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“…To minimize sample preparation and accelerate analysis, a variety of ambient ionization platforms have been developed, including a number of techniques involving spray desorption and liquid microjunction-based interfaces . One robust liquid microjunction-based platform is liquid extraction surface analysis (LESA), in which the extraction solvent is applied directly to the sample of interest, and the extracted analytes are subsequently introduced into the mass spectrometer using nano-electrospray ionization (nanoESI). The sensitivity, automated interface, solvent flexibility, and negligible carryover makes LESA particularly well suited for translational and clinical applications.…”

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confidence: 99%

In Vitro Liquid Extraction Surface Analysis Mass Spectrometry (ivLESA-MS) for Direct Metabolic Analysis of Adherent Cells in Culture

et al. 2018

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Conventional metabolomic methods include extensive sample preparation steps and long analytical run times, increasing the likelihood of processing artifacts and limiting high throughput applications. We present here in vitro liquid extraction surface analysis mass spectrometry (ivLESA-MS), a variation on LESA-MS, performed directly on adherent cells grown in 96-well cell culture plates. To accomplish this, culture medium was aspirated immediately prior to analysis, and metabolites were extracted using LESA from the cell monolayer surface, followed by nano-electrospray ionization and MS analysis in negative ion mode. We applied this platform to characterize and compare lipidomic profiles of multiple breast cancer cell lines growing in culture (MCF-7, ZR-75–1, MDA-MB-453, and MDA-MB-231) and revealed distinct and reproducible lipidomic signatures between the cell lines. Additionally, we demonstrated time-dependent processing artifacts, underscoring the importance of immediate analysis. ivLESA-MS represents a rapid in vitro metabolomic method, which precludes the need for quenching, cell harvesting, sample preparation, and chromatography, significantly shortening preparation and analysis time while minimizing processing artifacts. This method could be further adapted to test drugs in vitro in a high throughput manner.

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“… 10 Chip-based infusion nanospray ionization system has been described as liquid extractive surface analysis (LESA). 2 Walworth et al stated a lower limit of detection (LLOD) of 0.1 ng for propranolol using LESA with SRM detection, with extraction efficiencies of up to 77% reported for samples on a stainless steel plate. 18 …”

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confidence: 99%

“…Analysis of surfaces has exploited mass spectrometry as a versatile detection system for many years. Extractive sampling of surfaces by direct contact of a liquid interfaced to electrospray ionization mass spectrometry (ESI-MS) − is highly attractive as it can provide continuous monitoring and potentially high sensitivity for targeted compounds. Further downstream chromatographic separation could be applied to complex samples.…”

mentioning

confidence: 99%

“…Operating at a flow rate of 15 μL/min with an aqueous/methanol mixture, it was assessed to have quantitative capability, a limit of detection (LOD) of 50 ng/mL by selected reaction monitoring (SRM), for drugs in dried blood spots and thin tissue sections . Chip-based infusion nanospray ionization system has been described as liquid extractive surface analysis (LESA) . Walworth et al stated a lower limit of detection (LLOD) of 0.1 ng for propranolol using LESA with SRM detection, with extraction efficiencies of up to 77% reported for samples on a stainless steel plate …”

mentioning

confidence: 99%

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Electro-Focusing Liquid Extractive Surface Analysis (EF-LESA) Coupled to Mass Spectrometry

Brenton

Godfrey

2014

Anal. Chem.

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Analysis of the chemical composition of surfaces by liquid sampling devices interfaced to mass spectrometry is attractive as the sample stream can be continuously monitored at good sensitivity and selectivity. A sampling probe has been constructed that takes discrete liquid samples (typically <100 nL) of a surface. It incorporates an electrostatic lens system, comprising three electrodes, to which static and pulsed voltages are applied to form a conical “liquid tip”, employed to dissolve analytes at a surface. A prototype system demonstrates spatial resolution of 0.093 mm2. Time of contact between the liquid tip and the surface is controlled to standardize extraction. Calibration graphs of different analyte concentrations on a stainless surface have been measured, together with the probe’s reproducibility, carryover, and recovery. A leucine enkephalin-coated surface demonstrated good linearity (R2 = 0.9936), with a recovery of 90% and a limit of detection of 38 fmol per single spot sampled. The probe is compact and can be fitted into automated sample analysis equipment having potential for rapid analysis of surfaces at a good spatial resolution.

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Liquid Extraction Surface Analysis (LESA): A New Mass Spectrometry‐Based Technique for Ambient Surface Profiling

Cited by 3 publications

References 35 publications

Direct Coupling of Dispersive Extractions with Magnetic Particles to Mass Spectrometry via Microfluidic Open Interface

Direct Coupling of Dispersive Extractions with Magnetic Particles to Mass Spectrometry via Microfluidic Open Interface

In Vitro Liquid Extraction Surface Analysis Mass Spectrometry (ivLESA-MS) for Direct Metabolic Analysis of Adherent Cells in Culture

Electro-Focusing Liquid Extractive Surface Analysis (EF-LESA) Coupled to Mass Spectrometry

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