Pacific Northwest National Laboratory, Clemson University
Abstract
A new, multi-electrode, liquid sampling glow discharge ionization source for mass spectrometry is described. This ion source consists of multiple (2–4) counter (anode) electrodes in comparison to prior single counter electrode designs of this type. In the experiments presented here these ion sources have been interfaced with ThermoScientific Exactive Orbitrap instruments and Advion Interchim Scientific® expression® Compact Mass Spectrometer (CMS) instruments. Advantages and analytical performance improvements are described. These include the ability to use higher plasma currents, resulting in a more robust and energetic plasma exhibiting higher sensitivity, lower spectral background, ppt detection limits, and 2–3× faster washout times. A low-cost, 3D printed version of a dual counter electrode design is also described. The ion source can further be utilized in either atomic (elemental/isotopic) or molecular (molecular ion, fragmentation) ionization modes.
This is one from a set of two application notes. In this application note, we determine the purity of collection of a small (0.2%) impurity in a concentrated sample mix by mass-directed fraction collection using supercritical fluid chromatography (SFC) coupled with the Advion expression Compact Mass Spectrometer (CMS).
For the other application note on the recovery and purification of two, three component standard mixtures, click here.
Advion co-authored with a major pharmaceutical partner to create two application notes highlighting the benefits of supercritical fluid chromatography (SFC) coupled to a compact mass spectrometer for mass directed fraction collection. These application notes conclude that mass‐directed fraction collection with a simplified passive splitter on the Preparative JASCO SFC coupled with expression CMS system increases purification selectivity by mass directed fraction collection while maintaining excellent recovery and purity. The MS accepted high concentrations of sample material with peak shapes trailing edges almost indistinguishable from the UV trace. Low, Middle and High isocratic flow rates all showed comparable MS source clearance leading to minimal tailing beyond the UV. Gradients further minimized peak tailing as expected on the UV and this was also seen on the TIC and XIC. Peak purities for all main band purifications were ≥99.9% pure and minor impurity collections showed equivalent success yielding 100% pure fractions. Acceptable recoveries for all collected fractions were 94% or better.
A simple, sensitive and selective ASAP® sample introduction approach to measuring the presence of two isobaric compounds, CBDA and THCA, contained in a complex sample such as hemp or cannabis plants or their corresponding extraction products. Measurements are made of differences in the relative composition of CBDA and THCA fragment ions originating from the same precursor ion. Applicability to screening plants and plant product materials such as hemp or marijuana to monitor out-of-specification composition is demonstrated.
This application was developed from the poster presented at the 2018 Cannabis Science Conference in Portland, OR.
The combination of the Advion Interchim Scientific expression® CMS and puriFlash®flash chromatography technologies speed up the synthesis, purification and characterization of a compound.
Using the Advion Interchim Scientific expression®Compact Mass Spectrometer, the Plate Express™ TLC Plate reader, the ASAP® Atmospheric Solids Analysis Probe, and the puriFlash®XS520 flash purification system, it is now possible to execute a fast, user-friendly workflow to run TLC, harness the power of your cell phone to develop a flash method, and finally utilize a simple dipping probe to confirm fractions in seconds.
With easy sampling techniques, intuitive software, and advanced detection technology, you can easily and confidently synthesize, purify and characterize your compound, in a flash.
The collection of solid particulates and liquids from surfaces by the use of cloth swipes is fairly ubiquitous. In such methods, there is a continuous concern regarding the ability to locate and quantitatively sample the analyte species from the material. In this effort, we demonstrate the initial coupling of an Advion Plate Express plate reader to a liquid sampling–atmospheric pressure glow discharge (LS-APGD) microplasma ionization source with an Orbitrap mass spectrometer to perform uranium isotopic analyses of solution residues on cotton swipes. The Plate Express employs a sampling probe head to engage and seal against the swipe surface. Subsequentially, the analyte residues are desorbed and transported within a 2% HNO3 electrolyte flow to the ionization source. Quantitative recoveries were observed following a single 30 s extraction step, with the absolute mass sampled per extraction being ∼100 ng. While the intrasample variability in the analytical responses for triplicate sampling of the same swipe yield ∼30% RSD, this lack of precision is offset by the ability to determine isotope ratios for enriched uranium specimens with a precision of better than 10% RSD. Pooled, intersample precision (n = 9) was found to be <5%RSD across the various sample compositions. Finally, 235U/238U determinations (ranging from 0.053 to 1.806) were accurate with errors of <10%, absolute. The 234U- and 236U-inclusive ratios were determined with similar accuracy in enriched samples. While the driving force for the effort is in the realm of nuclear nonproliferation efforts, the ubiquitous use of cloth swipes across many application areas could benefit from this convenient approach, including the use of versatile, reduced-format mass spectrometer systems.
Mass spectrometric techniques are typically divided into two distinct fields: atomic and molecular. Liquid sampling – atmospheric pressure glow discharge (LS-APGD) has been developed as a versatile ionization source capable of combined atomic and molecular (CAM) analysis. To date, the LS-APGD has demonstrated impressive results in U isotope ratio analysis as well as molecular analysis across a wide range of instrument platforms.1-3 While molecular sampling has been demonstrated on this source, these samples fall into the realm of ESI-type samples, larger, polar compounds, most commonly LC-relevant drug targets. Presented here will be the demonstration of the wider versatility of the LS-APGD as a CAM ionization source using the Advion expression Compact Mass Spectrometer (CMS).
Authors: Tyler Williams1, Jacob R. Bills1, Jamey Jones2, and R. Kenneth Marcus1 1Clemson University, Department of Chemistry, Clemson, SC 29634 2Advion Inc, Ithaca, NY 14850
This poster was presented at the ASMS 2020 Reboot.
Dr. Jack Henion presents the possibility of using the Advion Interchim Scientific expression® Compact Mass Spectrometer (CMS) for ‘roadside breath testing’ of THC DRUID (driving under the influence of drugs) with the use of a small plastic breath collection device from Breath Explor of Uppsala, Sweden. This device serves as a simple, acceptable collection device for individuals in contrast to venous puncture with a needle or other means of collecting a biological sample.
In this ASMS 2020 Reboot presentation, you will learn:
Breath sample collection with the Breath Explor device
The potential benefits and challenges of a roadside LC/CMS testing system including an automated robot for sample preparation with the Advion Interchim Scientific expression® CMS and Advion Interchim Scientific AVANT UHPLC
The Advion LC/CMS system provides accurate and sensitive results when used to analyze breath samples for THC
Authors: Olof Beck2, Jack Henion1, Sabina Seferaj2, Peter Stamback3 1Advion, Inc., Ithaca, NY 2Karolinska Institute, Stockholm, Sweden 3Breath Explore, Munkplast AB, Uppsala, Sweden
Patulin is a mycotoxin that is a common contaminant in food and animal feed, especially in apple products. The potential health risk of patulin to humans led to the establishment of action levels in foodstuffs.
The EU, WHO and US FDA defined maximum levels of patulin in fruit juices. The EU also has specific regulations for solid apple products and foods intended for infants and young children such as apple compote.
In this application note, a simple UHPLC/CMS method using the Advion Interchim Scientific AVANT® UHPLC and expression® Compact Mass Spectrometer (CMS) system is introduced for the analysis of patulin in apple juice and apple compotes.
The research presented in this application note was a poster presentation for ASMS 2020 Reboot.
Patulin is a mycotoxin that is a common contaminant in food and animal feed, especially in apple products.The potential health risk of patulin to humans led to the establishment of action levels in foodstuffs.
The EU, WHO and US FDA defined maximum levels of patulin in fruit juices. The EU also has specific regulations for solid apple products and foods intended for infants and young children such as apple compote.
In this poster, a simple UHPLC/CMS method using the Advion AVANT UHPLC and expression Compact Mass Spectrometer (CMS) system is introduced for the analysis of patulin in apple juice and apple compotes.
This poster was presented at the ASMS 2020 Reboot.
The compound synthesis, purification and confirmation process often presents challenges throughout. From ensuring successful synthesis of your product, setting up a flash purification method, and finally confirming ID of fractions, the lengthy work flow can be time consuming and repetitive.
In this application note, we demonstrate how the combination of Advion Interchim Scientific technologies speed up the synthesis, purification and characterization of a compound.
This series features the Advion Interchim Scientific expression® Compact Mass Spectrometer (CMS), the Plate Express™ TLC Plate Reader, the Atmospheric Solids Analysis Probe (ASAP®), and the puriFlash® XS520 flash purification system.
