Advion’s expression® CMS paired with the Atmospheric Solids Analysis Probe (ASAP®) can quickly and easily be used to screen an unidentified drug mixture in this mobile field testing dramatization.
Fluorine-18 Labeled Fluorofuranylnorprogesterone ([18F]FFNP) and Dihydrotestosterone ([18F]FDHT) Prepared by “Fluorination on Sep-Pak” Method
National Institutes of Health
National Heart, Lung, and Blood Institute, National Cancer Institute
Abstract
To further explore the scope of our recently developed “fluorination on Sep-Pak” method, we prepared two well-known positron emission tomography (PET) tracers 21-[18F]fluoro-16α,17α-[(R)-(1′-α-furylmethylidene)dioxy]-19-norpregn-4-ene-3,20-dione furanyl norprogesterone ([18F]FFNP) and 16β-[18F]fluoro-5α-dihydrotestosterone ([18F]FDHT). Following the “fluorination on Sep-Pak” method, over 70% elution efficiency was observed with 3 mg of triflate precursor of [18F]FFNP. The overall yield of [18F]FFNP was 64–72% (decay corrected) in 40 min synthesis time with a molar activity of 37–81 GBq/µmol (1000–2200 Ci/mmol). Slightly lower elution efficiency (~55%) was observed with the triflate precursor of [18F]FDHT. Fluorine-18 labeling, reduction, and deprotection to prepare [18F]FDHT were performed on Sep-Pak cartridges (PS-HCO3 and Sep-Pak plus C-18). The overall yield of [18F]FDHT was 25–32% (decay corrected) in 70 min. The molar activity determined by using mass spectrometry was 63–148 GBq/µmol (1700–4000 Ci/mmol). Applying this quantitative measure of molar activity to in vitro assays [18F]FDHT exhibited high-affinity binding to androgen receptors (Kd~2.5 nM) providing biological validation of this method.
Analysis was performed by Select Ion Monitoring (SIM) and LC/MS using the Advion expression Compact Mass Spectrometer (CMS).
Innovations in Mass Spectrometry – Peak Express Software
During this webinar you will learn more about:
- A new type of mass spectrum: the Delta Spectrum (ΔS). The patented ΔS is able to look beyond chemical noise and automatically detect even the smallest peaks without knowing the m/z.
- How to easily find adducts, dimers, fragments, side-reactions and other unexpected compounds at the click of a button, in real-time or with post-processing.
- How to use Peak Express software to highlight minor components in complex mixtures and dirty matrices, and can give you the ability to control mass-directed purification without providing the compound mass.
- How to easily acquire XIC-quality data while scanning the entire mass range, allowing Peak Express™ to tell you the m/z.This webinar was featured by Lab Manager’s Tech Trends webinar series, “Innovations in Mass Spectrometry.”
Compact Mass Spectrometry: A Complete Reaction Monitoring Solution
Reaction monitoring is a key aspect in a range of chemistry environments from chemical synthesis to drug discovery to understanding natural products to protein synthesis. Understanding the optimal time to quench a reaction for maximum yield, as well as monitoring a reaction in real-time is vital to many medicinal and synthetic organic chemists. Advion Interchim Scientific’s expression® CMS was developed with the chemist in mind to optimize their workflow directly at the bench. It is an easy-to-use and maintain single quadrupole detector that integrates with the industry’s broadest range of innovative sampling techniques from direct probe analysis to ultra-high performance liquid chromatography. Users can rapidly switch between the many different sampling techniques required throughout the chemist’s workflow.
University of Minnesota, Therapeutics Discovery Development
Q: WHAT IS THE FOCUS OF YOUR LAB’S RESEARCH?
We are the Institute for Therapeutics Discovery & Development. One of our main research core’s goals is the synthesis of biologically active small molecules with the additional goal of training the next generation of scientists through the Department of Medicinal Chemistry’s graduate student program. Our projects focus areas include contraception, cancer, infectious disease, and Alzheimer’s.
Q: WHAT WAS YOUR PREVIOUS WORKFLOW OR CHALLENGES?
A major headache for any synthetic chemist is the identification of the desired product when a mixture is obtained from a reaction. In the past, we would typically run a flash chromatography column, isolate spots of potential interest, concentrate them, and take 1H NMR, sometimes having to go back to column fractions as many as 4 times to analyze new spots if the first wasn’t desired product.
Q: WHY DID YOU INCORPORATE THE expression® CMS INTO YOUR LABORATORY?
Advion’s TLC–CMS system has streamlined our purification and analytical process significantly. What once took several hours to days to complete, we can now accomplish in as a little as 60 seconds. The Data Express software is also very easy to work with and has been quite useful in identifying adducts of our compounds.
Q: WHO WOULD YOU RECOMMEND TO PURCHASE THE expression® CMS?
We have been extremely happy with our Advion system and predict that it will quickly become a workhorse in any synthetic organic or medicinal chemistry laboratory.
Teaching Mass Spectrometry For Chemists
Bring mass spectrometry into your classroom for remote or on-site learning with a training course for the expression® Compact Mass Spectrometer (CMS).
Advion offers an affordable MS teaching package that includes:
- A compact, easy-to-use benchtop mass spectrometer for both students and researchers
- Recorded lectures and video lab content
- Lecture slides to share or adapt to your own teaching style
PLUS: Easy, student-friendly software. Select the workflow, the type of compounds, and students are on their way with just a few clicks of the mouse.
A research-grade mass spec, the expression® CMS is ideal for teaching because of its small size, ease of use, and one-click software. When class is not in session, the system is ready for research, making this a versatile choice for university labs seeking state of the art equipment paired with streamlined teaching modules.
ASAP® Atmospheric Solids Analysis Probe
For Direct Mass Analysis of Liquid & Solid Samples with the expression® CMS
The direct atmospheric solids analysis probe, otherwise known as ASAP®, permits chemists fast and reliable sample analysis of liquid and solid samples such as reaction mixtures, food samples, natural products and tablets.
Chemists simply dip the closed end of a glass capillary into the sample of interest (even complex mixtures) or scrape the surface of a solid, and then place the capillary into the CMS for analysis.
Clean-up and analysis is a single step. Involatile buffers and salts remain on the capillary ensuring they do not suppress ionization or interfere with the measurement, while the compounds of interest are identified by the CMS.
In addition, users benefit from solvent-free APCI, which ionizes a wider range of compounds.
Plate Express®: Direct Mass Analysis from TLC Plates
Provides simple, automated MS analysis in seconds, directly from TLC plates
The Plate Express® is a device that provides a simple, automated means of obtaining mass spectra directly from TLC plates, creating a technique known as TLC/MS. Combined with Advion Interchim Scientific’s expression® compact mass spectrometer (CMS) this becomes TLC/CMS. Using this technique, chemists can quickly and confidently identify products even in complex mixtures without additional sample preparation.
- Identify spots in <1 minute
- Avoid the risk of overloading the mass spectrometer – TLC spots contain the ideal amount of sample for mass spectrometry
- Software controlled – spectra obtained within a few mouse clicks
- Simplify the process of obtaining spectra – ideal for multi-user labs
iASAP Inert Atmospheric Solids Analysis Probe
For Direct Mass Analysis of Air-Sensitive Samples, Catalysts and Organometallics at the Bench With the expression® CMS
The Atmospheric Solids Analysis Probe (ASAP®) allows chemists to directly analyze liquid and solid samples by mass spectrometer without the need for sample preparation at the bench, right next to the reaction. The inert ASAP (iASAP) is a modification of this technique, allowing easy sampling of air-sensitive compounds, such as metal catalysts and organometallics, from reactions that are carried out in a glove box or Schlenk line to prevent oxidation.
The technique allows a synthetic chemist to perform real-time reaction monitoring by sampling the compound with the special iASAP probe, which is designed to provide access to a sample protected in a glovebox or Schlenk line, then transferring the sample to the CMS, while continuing to protect it in an inert environment where it is ionized by atmospheric pressure chemical ionization (APCI). Mass Spectra are acquired in seconds.
AVANT® HPLC & (U)HPLC Chromatography Systems
Providing simple, high-performance, LC/CMS with the expression® CMS
Modular, stackable design, with many options provides custom solutions for both HPLC and UHPLC needs. From the simplest manual injection HPLC to a fully automated, streamlined UHPLC system and everything in-between, the Avant series can be configured to fit your analytical requirements and your budget.
The AVANT® (U)HPLC series is the latest in Advion’s innovative line of sample inlet devices for the expression® CMS which include:
- Plate Express® for automated mass assays from TLC plates
- The ASAP® direct analysis probe for solid, liquid and even air sensitive samples using iASAP
- vAPCI for analysis of volatile organic compounds (VOCs) from head spaces, breath, and other gas samples.
- Flow chemistry interfaces
All these techniques can be simply, simultaneously, interfaced with the CMS so that the chemist can move quickly and effortlessly between workflows.