Teaching Mass Spectrometry in the Laboratory

Mass spectrometry is becoming more prevalent. As the applications for and use of mass spectrometry continue to increase, so will the number of careers that need knowledge of these tools.

In the past, a high number of undergraduate students graduated with a chemistry degree without ever coming into contact with a mass spectrometer.

Chemistry students had to reconcile this absence by learning the principles of mass spectrometry in a lecture room and giving samples to a technician for investigation when in the teaching laboratory.

The international mass spectrometry market is estimated to increase by 7.6% annually, to reach a worth of over $10.5 billion by 2025, as stated on a recent report by the Market Research Engine.1

All these new instruments must be built, maintained, and designed, and their users will need to comprehend the data and know-how to get the best results from the equipment.

As a result of the declining cost and size of mass spectrometers, along with their increasing ease of use and robustness, universities are now beginning to supply their undergraduate chemistry laboratories with this pioneering analytic tool.

My favorite learning environment in the laboratory,” states Paul A. Flowers, Professor of Analytical Chemistry at the University of North Carolina at Pembroke. He continued, “I like teaching students fundamentals through bona fide research experiences.

Flowers started employing mass spectrometry in the teaching laboratory around six years ago and has not looked back.

In the present day, a growing petrochemical industry, increased pharmaceutical R&D spending, and a governmental focus on drug safety, food quality, and environmental testing are all important contributors to the continued growth of mass spectrometry.

The latest applications for mass spectrometry, such as those in homeland security, clinical diagnostics, and the legal cannabis market, are promoting further development, as is the requirement for chemical analysis in remote locations, even in outer space.

Through practical experience with instruments, “Students learn how the data is generated and not to just take it at face value,” says Blánaid White, Associate Professor in Analytical Chemistry at Dublin City University in Ireland, “They also gain a better understanding of the fundamentals.

Training Future Analytical Chemists

Mass spectrometry is a workhorse in a range of environments, from law enforcement to the pharmaceutical industry.

To offer a taste of this variety, Flowers trains students in his senior-level courses to utilize mass spectrometry in identifying unknown explosives and the active ingredients in medications.

His teaching laboratory showcases an Advion expression® Compact Mass Spectrometer (CMS) and a direct analysis probe called the ASAP® (atmospheric solids analysis probe).

The probe employs atmospheric pressure chemical ionization (APCI) of the instrument, which removes the requirement for students to perform any sample preparation before investigation.


A schematic of the Atmospheric Solids Analysis Probe (ASAP). Image Credit: Advion.

The Advion expression CMS is a super nice instrument,” Flowers states, “The APCI ion source with an ASAP sampling probe allows for direct insertion of liquids and solids, making for very quick analyses.

Every analysis normally takes 30 seconds or less. “In our larger-enrollment, lower-level labs, we can get a lot of students in and out quickly,” he explains. The students employ the instrument to determine the active ingredients in painkillers accessible over-the-counter.

As an example, a migraine medication, “has three easily identified components—caffeine, acetaminophen, and aspirin,” Flowers states.

An easily identified peak for acetaminophen was found using a positive ion ASAP/ CMS analysis of a tablet.

Example 1. An easily identified peak for acetaminophen was found using a positive ion ASAP/ CMS analysis of a tablet. Image Credit: Advion.

The students utilize the same arrangement to analyze an unknown explosive on a fragment of glass. Spectra are gathered from four standards: the explosives nitroglycerin, pentaerythritol tetranitrate (PETN), hexahydro-1,3,5-trinitro-1,3,5- triazine (RDX), and 2,4,6-trinitrotoluene (TNT), which are contrasted with the unknown explosive’s spectra.

Similar to the acetaminophen example, an explosive compound such as RDX is easily detected when using the ASAP/CMS analysis method. For the full application note, read “Screening of Explosive Residues without Sample Preparation Using a Direct Sample Analysis Probe on the expression CMS.”

Example 2. Similar to the acetaminophen example, an explosive compound such as RDX is easily detected when using the ASAP/CMS analysis method. For the full application note, read “Screening of Explosive Residues without Sample Preparation Using a Direct Sample Analysis Probe on the expression CMS.” Image Credit: Advion.

To allow the students to research deeper into mass spectrometry itself, Flowers performs an experiment focused on instrumentation that acquaints the students with the fundamental concepts of mass spectrometry.

This class employs caffeine as its test substance and examines electron ionization (EI) mass spectrometers.

The students experiment firsthand with the two kinds of ionization sources, APCI and EI, researching the influence of a range of instrumental parameters on spectral quality.

Students are also able to perform more detailed research projects utilizing the expression CMS.

Students in our instrumental analysis course spend several weeks working on individual lab projects. One recent project explores the use of internal standards to improve the precision of ASAP measurements,” Flowers explains.

Projects such as these put the entire spectrum of mass spectrometry testing, calibration, sampling, and maintenance directly into the hands of the students.

Third-year analytical science students at Dublin City University gain practical experience with a gas chromatography/mass spectrometry (GC/MS) instrument.

Experiments entail the discovery of hydrocarbon pollutants in soil samples and the comparison of branded and generic nonsteroidal anti-inflammatory drugs. The students from Dublin also learn mass spectrometry essentials such as methods for sample preparation that enhance the data acquired by the tool.

They compare a couple of derivatization agents and see how that what they do to a sample as part of its pretreatment can have such a massive impact on the signal that is generated at the end,” White states.

Then in their final year, because they’ve got the experience and the training on it in third year, our students have a suite of instrumentation available to them to use during a research project,” she says.

Dublin City University’s analytical science students typically gain employment in the pharmaceutical industry. “In Ireland, we have a huge number of the big pharma companies with manufacturing plants. So a lot of our students do go directly into those plants,” White explains.

The students achieve roles such as production chemists, quality control analytical chemists, and process chemist.

At Wilkes University, students majoring in Chemistry utilize an expression CMS as part of an investigation created to provide them with practical experience of validating a high-performance liquid chromatography (HPLC) column.

HPLC column manufacturers supply certificates that report the elution times of particular compounds, under specific conditions. It is essential that users evaluate the performance of their columns against the claims of the manufacturer, to verify correct analyses.

Undergraduate student Jose Acosta, University of North Carolina, using the expression CMS to investigate the precision of the ASAP probe for analyzing aqueous caffeine.

Undergraduate student Jose Acosta, University of North Carolina, using the expression CMS to investigate the precision of the ASAP probe for analyzing aqueous caffeine. Image Credit: Paul Flowers.

I want my students who leave here and go to work for industry to understand that you need to periodically evaluate the column performance.

Donald E. Mencer, Associate Professor of Analytical Chemistry at Wilkes University

In his laboratory, the 300-level students prepare samples, including four or five components. “We’ve got a small post-HPLC column splitter valve that after the sample runs through the HPLC column we split about 0.8 mL/min to the UV detector and the other 0.20 mL/min to the mass spec detector,” Mencer describes.

He added, “They collect data in both data channels and learn a little bit about the different sensitivity of the mass spec detector and that not all molecules ionize equally efficiently.

For this investigation, the students are utilizing an electrospray ionization source on the expression CMS. For undergraduate research projects, Wilkes University also has an ASAP that is used for this purpose.

It’s pretty easy to switch the electrospray ionization source that we tend to use when it’s hooked up to the HPLC over to the APCI if we want to use the ASAP probe. It only takes a few minutes,” Mencer states.

One of the things I like about the CMS is that it’s not intimidating at all to students. You can pretty quickly get them past any initial fears about picking apart hardware and putting in pieces and reconfiguring the plumbing,” he explains.

Training Prospective End Users

Mass spectrometers are additionally beginning to be applied in organic chemistry teaching laboratories as a frequent tool for establishing the identities of synthesized molecules.

When a student acquires data that is unclear from infrared and nuclear magnetic resonance (NMR) spectroscopy for their synthesized product, “We can now say, ‘Let’s put it on the mass spec and see if we can find any of your compound in your mixture,’” states Andrew Worrall, Deputy Director of Chemistry Teaching Laboratories at the University of Oxford, UK.

From deciding we want to do it to getting the results takes a couple of minutes,” he adds. The University of Oxford in September 2018 launched new chemistry teaching laboratories with an analytical suite estimated to cost several million pounds.

It has an expression CMS, along with other advanced instruments, for example, a benchtop NMR spectrometer. Oxford students employ an ASAP to verify the identity of molecules.

The latest analytical suite is also furnished with a Plate Express™ TLC (thin-layer chromatography) Plate Reader for the expression CMS; this arrangement is frequently called TLC/CMS. In under a minute, this arrangement acquires mass spectrometry data from a spot on a developed TLC plate.

In seconds, the TLC/CMS system can run an additional sample. “We use the TLC mass spec in an experiment where students extract caffeine from a natural product, like tea,” Worrall explains.

The students do a crude extraction, run a TLC on the crude extract, and then use the TLC mass spec to identify which part of the TLC contains caffeine.” From this, they can enhance the design of the purification step.

The Plate Express TLC plate reader for the expression CMS collects mass spectrometry data from a spot on a developed TLC plate.

The Plate Express TLC plate reader for the expression CMS collects mass spectrometry data from a spot on a developed TLC plate. Image Credit: Advion.

This experiment is an example of the movement away from the conventional ‘cookbook’ methodology in teaching laboratories.

We’re moving away from telling students to follow a recipe, where they are basically technicians. We want to train them to become research scientists.

Malcolm Stewart, Director of Teaching Laboratories in the Department of Chemistry at Oxford.

Introducing undergraduates to expensive pieces of [equipment] also gets them ready for the high-tech environment during their fourth-year research project with one of our research groups,” Worrall explains.

At Purdue University, the college of pharmacy also supplied a TLC/CMS for its undergraduate organic chemistry laboratory in the fall of 2018. The university already had three in use for research, and this was the fourth expression CMS purchased.

The expression CMS ASAP probe allows for the direct insertion of liquids and solids, with no sample preparation required.

The expression CMS and ASAP probe allows for the direct insertion of liquids and solids, with no sample preparation required. Image Credit: Advion.

When I saw the user-friendly interface, how quickly data was collected and how easy it was to analyze the data, I thought it was the easiest mass spec that I’d ever used.

Daniel P. Flaherty, Assistant Professor of Medicinal Chemistry at Purdue University.

Flaherty additionally thought that TLC/CMS could be beneficial in improving the understanding of undergraduates regarding both mass spectrometry and compound characterization in organic chemistry, he explains.

Students were previously handed printouts of mass spectrometry data and were asked to explain to their instructors what the molecule was. “Now, they can go and collect their own data on the molecule,” Flaherty states.

Purdue students evaluate the data on the instrument itself at present, but there are plans to allow for the data to be remotely accessed using the Advion Data Express processing software, because each student can access and download the software from his or her personal computer.

A system is already in place in the department that is utilized with different analytical instruments. “The students use the instrument to collect the data, put the data on a flash drive, and then take it back to their workstation and analyze it there,” Susan R. H. Holladay states.

Holladay is the Director of Undergraduate Laboratories at Purdue. She says, “That is the model that we’re going to use for the Advion mass spec next time we teach with it.” Purdue began to utilize TLC/CMS last year in a nitration study for sophomores in the teaching laboratory.

The reason we found the need for the TLC plate reader with this nitration experiment is because the products can be nitrated more than once,” she explains.

Infrared analysis and melting points of the product has not always provided a clear answer regarding the obtained product in the past.

By using the mass spec, they can quickly and clearly see what the mass of their product is,” Holladay states. “One of the things that we work hard on is making sure that we don’t have just cookbook laboratories,” she says.

Holladay adds, “We don’t want the students to just show up, make a substance, verify the substance, and then go, ‘Oh, look, we made what we thought we made!’ We, therefore, give our students different starting materials. So, they’re doing the same experiment, but getting different products.

Holladay and Flaherty now intend to introduce the TLC/CMS to a range of different organic chemistry teaching laboratory studies which lack an objective answer about the identity of the product.

We try not to use an instrument just to use an instrument,” Holladay states. Holladay, Flaherty, and others attempt to ensure that its use is promoting the learning of students, she explains.

Looking to learn more about TLC/CMS? Download the application note, “Suzuki Reaction Monitoring Using Compact Mass Spectrometry with the Plate Express TLC Plate Reader.

Conclusion

Affordable compact mass spectrometers are predicted to continue their invasion into university teaching laboratories.

Their usability, robustness, and speed are allowing, for the first time in many cases, undergraduate students to gain practical experience with a research-grade instrument that they are more and more likely to encounter if they advance within a career in science.

The lessons gained from experiential education in mass spectrometry will remain with them every step of the way.

References and Further Reading

  1. Market Research Engine, Mass Spectrometry Market by Platforms Analysis (Hybrid Mass Spectrometry, Single Mass Spectrometry); by Application Analysis (Pharmaceuticals, Biotechnology, Industrial Chemistry, Environmental Testing, Food & Beverage Testing) and by Regional Analysis—Global Forecast by 2018- 2025 (Deerfield Beach, FL: Market Research Engine, December 2018), https:// www.marketresearchengine.com/mass-spectrometry-market.

This information has been sourced, reviewed and adapted from materials provided by Advion.

For more information on this source, please visit Advion.

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