Nominate a colleague or yourself for the 2022 

 Lifetime Achievement in Chromatography Award

 is seeking nominations for the 14th Annual Lifetime Achievement in Chromatography award, to be awarded in 2022. 

 Lifetime Achievement in Chromatography Award, as its name implies, recognizes a separation scientist for his or her overall contributions to the field of chromatography. The winner, chosen by an independent committee, will be featured on the cover of a 2022 issue of 

 and in an interview that will be featured in our electronic newsletter, e-Separation Solutions, and on the 

	A list of past winners can be found on the 


	To nominate a candidate, please use this 

to provide the information listed below about the person you are nominating.

	Please email the completed form to Laura Bush, the editorial director of 

		Candidate’s full name:           

		Current job title (if retired, please indicate that and include last known job title before retirement):      

		Area(s) of focus of work (maximum 200 words):      

		Short summary, in 100 words, of the candidate’s achievements or contributions (more details can follow in the sections below):      

		Please list the candidate’s most important contributions to the field of chromatography and explain briefly the significance of each (maximum 800 words):

		Number of oral and poster presentations at scientific conferences: 

		Service provided to the scientific community, such as volunteer work in scientific societies, organizing conferences, work as a journal reviewer, teaching short courses, mentoring young scientists, and so on. Please quantify where possible (e.g., number of students in short courses): 

	Nominations should be sent to Laura Bush, the editorial director of 

	Questions about the submission process should be directed to Laura Bush at 

	Please note that this call for nominations is for the 2022 award

Articles

2022 Lifetime Achievement in Chromatography Award Call for Nominations

Nominate a colleague or yourself for the 2022

 Emerging Leader in Chromatography Award  

 is seeking nominations for the 14th Annual Emerging Leader in Chromatography award, to be awarded in 2022.  

 Emerging Leader in Chromatography award recognizes the achievements and aspirations of a talented young separation scientist who has made strides early in his or her career toward the advancement of chromatographic techniques or applications. The winner will be featured on the cover of a 2022 issue of 

	A list of past winners can be found on the 

 Emerging Leader in Chromatography award must work in the field of separation science. In 2022, candidates must be within 10 years of receiving their highest degree, and must have made significant practical contributions to the field of separation science that have helped advance the state of the art in the fundamentals or application of chromatography. Weight will be given to candidates who have taken a leadership role at their university, institute, or place of business. 


	You may nominate a colleague or yourself. To nominate a candidate, please email the following documents to Laura Bush, the editorial director of 

1. INFORMATION ABOUT THE PERSON YOU ARE NOMINATING 

, please provide the following information about the person you are nominating:

		Year highest academic degree was earned and from where (list degree, year, institution, and location). 

Important: Candidates must be within 10 years of receiving their highest degree in the year the award is presented.

		Short summary, in 100 words, of the candidate’s achievements or contributions (more details can follow in the sections below)

		Please list the candidate’s five most important pieces of work (such as papers in peer-reviewed journals, technical reports written in an industrial community, patents, or other) and explain briefly the significance of each. 

		Other key contributions to the field of separation science not captured above

		Number of oral and poster presentations at scientific conferences


	Please include a maximum of two letters of support from members of the separation science community. (Additional letters will not be considered during the voting process.) Information in the supporting letters should complement, not repeat, the information contained in the nomination form.


	Please provide a current resume or CV of the candidate in a Word or PDF file.


	Include a high-resolution headshot of the nominee in a .JPG format.

	Submissions should be sent to Laura Bush, the editorial director of 

	Questions should be directed to Laura Bush at 

	Please note that this call for nominations is for the 2022 award. 

2022 Emerging Leader in Chromatography Award Call for Nominations

Q. What trends do you see emerging in GC or GC–MS?

The global trends we are seeing and working on with our customers are a desire for miniaturization, flexibility, and faster results. For example, full automatization of sample preparation and multiple detection channels are helping to address the need for more specific and confident results with shorter turnaround times.

In the areas of food safety and environmental health, the number of samples as well as regulatory requirements are always increasing, so this demands a focus on targeted and non‑targeted molecules.

User-friendly data handling solutions that are combined with smart instruments and approaches, including artificial intelligence, are helpful in preventive maintenance, lowering the cost of ownership, and simplifying workflows—essentially bringing turnkey solutions for QA/QC or analytical laboratories.

One trend is the development of smart connected functionality to improve and streamline the user experience. Functions, such as automatic leak checks and troubleshooting diagnostics, allow operators to achieve better results faster, with fewer mistakes. Also, proactively guiding users through preventative maintenance steps helps reduce unplanned downtime and sample reruns, greatly improving productivity.

There is a clear trend to cross‑train operators and a requirement for them to stay connected with what’s happening in several laboratories simultaneously, even when they are not physically in any given one. Remote connectivity is a future trend as an “Industry 4.0” digital transformation sweeps across analytical laboratory enterprises worldwide, driving resource deployment optimization. Smart functionality and remote connectivity are also invaluable when optimizing laboratory operations during a pandemic, especially when laboratory access is limited.

Green chemistry and sustainable operations are also clear trends, and many new instruments are being designed to use less power, water, helium, and other natural resources. We are seeing increased use of recently introduced, cost-efficient, oil-free GC–MS pumps, that run much quieter and cleaner, and eliminate oil spills. Moving applications to smaller, greener, and faster GC systems with efficient direct heating technology, is also a growing trend.

We are seeing an increase in discovery-based approaches, where workflows that are typically seen in the “omics” fields are now expanding to other application areas. Analysts no longer want to simply comply with regulated methods, but also want to see what else is present in their samples. For example, in the automotive industry, manufacturers must adhere to Vehicle Interior Air Quality (VIAQ) regulations, but now also want to be able to monitor other potentially harmful compounds and those which may contribute to malodours.

Recent emerging trends in GC and GC hyphenated with MS include an increase in the use of mass spectrometers, especially triple quadrupole instruments, instrument miniaturization, and the migration towards multiclass methods of analysis. The upward trend in the adoption of triple quadrupole instruments is a result of the increased sensitivity and selectivity requirements of challenging multiclass methods, improvements in MS sensitivity, and the reduction in MS pricing. In some cases, detector sensitivity is outpacing instrument and analytical column designs, which should prompt further research and subsequent improvements. Miniaturization of instruments, and the trend toward “black-box” applications continue to surface. These instruments are generally intended to cater to field applications and highly routine operations.

There is still work to be done around capabilities for increasingly lower detection limits and in the chromatography process itself.

Miniaturization and the need for faster analysis is creating opportunities for chips technology or low thermal mass systems together with new micro-detectors and mass spectrometers.

Portable GC–MS with on-field sampling techniques is the most important growth driver in GC and brings immediate results in various fields such as air pollution or soil analysis.

In classical GC, we observe a global trend towards hyphenated technologies, such as thermal gravimetry combined with infrared (IR) and GC–MS, to characterize advanced materials and microplastics. This “best of both worlds” approach brings more information-rich data to scientists and technicians in a single run.

GC is not going away any time soon. While it is a mature technology, there are still many important applications that depend on GC, such as monitoring climate change, supporting petrochemical processing, and assuring purity of pharmaceuticals from residual solvent residues. However, especially for many food and environmental applications, the future will see more and more GC systems coupled to mass spectrometers. Notably, triple quadrupole GC–MS will be deployed more and more routinely.

In the future, micro-GC will continue to be valued for its convenient small form factor and rapid cycle times. This makes it ideal for “going to the sample”, for example in reaction gas monitoring—an application that is growing, especially as alternative biofuel research is increasingly funded. Also, as natural gas grows in popularity as a fuel source, micro-GC is being used more and more to verify calorific value as a measure of quality and economic valuation.

With the use of GC×GC becoming routine, we are seeing a resurgence in the use of single-channel detectors, such as the simple, robust flame ionization detector (FID) or highly sensitive and selective detectors like sulphur chemiluminescence detectors (SCD). Quality control laboratories that would have previously resorted to MS in an attempt to deconvolve complex samples now benefit from the enhanced separation of GC×GC coupled with single-channel detectors, while in discovery applications, parallel detection is on the rise for fully automated qualitative MS and quantitative FID workflows.

In the cannabis industry, the analysis of terpenes by GC–MS has been particularly problematic. The extreme diversity of the terpene and terpenoid classes, as well as their similar spectra, result in deconvolution difficulties and poor data quality, but physical separation by GC×GC allows confidence in results even with simple FID, as well as a wide dynamic range and robust quantitation.

The future of GC and GC–MS will continue to focus on platform miniaturization, reduced analysis times, increased sensitivity, and more rugged chemistries in the sample pathway. For example, electrical and mechanical advances will continue to reduce the size of GC ovens and MS detectors. Reduced analysis times will come by the way of shorter and/or narrower bore columns coupled with a more maintenance‑friendly option to thermally‑resistive column heating, a technology the market as a whole has been unwilling to adopt.

MS will continue to increase in sensitivity, such as lower detection limits, through more efficient generation and transfer of ions. Instrument uptime will be maximized through the development of more rugged surface chemistries and easily replaceable guard assemblies. We also expect to see greater adoption of tandem mass detectors as their price and footprint continues to drop.

Ultimately, the future of GC or GC–MS may be uncertain with the potential adoption of ambient/atmospheric pressure ion sources such as desorption atmospheric pressure photoionization (DAPPI), desorption electrospray ionization (DESI), and/or direct analysis in real time (DART). These ionization techniques are currently applied without the use of a GC system. The future is unclear as to whether or not these ionization techniques will be incorporated with the use of a GC or eliminate the need for a GC system. Until that time, instrument manufacturers will continue to innovate in all the aforementioned areas.

Q. What is the GC or GC–MS application area that you see growing the fastest?

This tends to depend on which geographies you are talking about. Emerging markets such as India or China see their regulations growing rapidly especially in air and water monitoring, and also in food quality due to globalization, so this is driving GC and GC–MS demand.

Furthermore, pharmaceutical companies have invested a lot in production plants (especially in China, India, and Israel to lower production costs) and require routine QA/QC systems under GMP-regulated environments.

In more mature markets, such as North America and Europe, cannabis and hemp markets also continue to be a growth enhancer for GC as well as food safety and QA/QC laboratories that are expanding their GC and GC–MS use faster than, say, the academic or R&D service areas.

High-throughput systems or fully automated sample handling devices are also in higher demand and generally GC–MS systems have become accepted as an important tool globally as a result of their more specific and sensitive detection capabilities and simplified use.

 Detecting nitrosamines in pharmaceuticals by GC–MS has grown sharply this past year as pharmaceutical companies race to assure their products are free of these contaminants.

Air and water quality continue to be recognized as critical, not only to human health, but also to the health of the planet as a whole. This is a growing application area especially in markets such as China and India. As new materials are developed and more commonly used, their presence in air and water are increasing. Detection of perfluorinated alkanes (PFAS) in water is a major growing concern. Microplastics finding their way into waterways and associated biota is also a rapidly growing area of research and regulation development. The recently approved US Senate Bill 1422 in the State of California specifies funding for developing analytical methods for measuring microplastics with an intention to set appropriate regulatory levels over the next several years.

The growing legalization of cannabis worldwide is driving rapid demand for purity and potency analysis. GC–MS Triple Quad (TQ) is an especially popular technique to determine pesticides in plant materials, and demand for this application is growing rapidly. Recent legalization of harvesting hemp as a multipurpose raw material is also driving a growing need to verify its authenticity and freedom from tetrahydrocannabinol (THC) using GC–MS.

An obvious one is the cannabis industry, and this is expected to increase further when regulated testing methods are enforced. We have also seen a rapid increase in biomarker discovery—from samples such as breath, urine, and saliva—in an effort to develop non‑invasive diagnostic tests.

Both application areas will benefit from the adoption of routine, robust, fully automated workflows that encompass everything from sample preparation to data handling and reporting. They deal with high numbers of samples, and automation could help to develop standardized approaches across these industries.

Emerging contaminants in the environment as well as the expanding legalization of cannabis are two areas that have seen growth and change in analytical approaches and techniques. While the risk to human health has not been determined for emerging contaminants, scientists and regulatory agencies support research to document these compounds, most notably in drinking water. Brominated flame retardants (BFRs) have gained notoriety given their ubiquitous use in products and persistence in the environment. While cannabis potency is best performed by LC, GC is most suitable for residual solvents and terpene analysis. Cannabis concentrate products such as tinctures, edibles, and oils are extracted in solvents and those products must be analyzed by GC to verify they are free of solvents prior to human consumption. Terpenes are a class of compounds responsible for the flavours and aromas in cannabis. Cannabis growers are interested in determining the ratio of terpenes in different strains for their possible therapeutic effects.

Q. What obstacles stand in the way of GC or GC–MS development?

We often say that virtually nothing is impossible in GC. Initially designed for small volatile and non‑polar molecules, recent column developments have brought GC and GC–MS into the extended application ranges of polar or larger molecules analysis. As an example, the recent development of thermally‑resistant polar stationary phases, such as ionic liquids, removes traditional barriers. Hence, GC development can no longer be considered in a silo and should be developed together within the application need—including consumables, sample matrix handling, and software solutions.

Many of the recent developments in GC have also brought specific solutions to specific needs or constraints in niche markets such as multidimensional analysis or LC–GC for mineral oil saturated hydrocarbons/mineral oil aromatic hydrocarbons (MOSH/MOAH) analysis.

From a GC-solution-provider standpoint like ours, there is no limitation around GC’s technical capabilities. The challenge is more around seeing research and development return on investment (ROI) for GC solutions that are created to address small/niche markets and realities around what customers are able and willing to invest in terms of innovation.

The ever‑increasing complexity of materials needing to be analyzed by GC or GC–MS poses a real challenge to technology and instrument development. Advanced composite materials are increasingly used in new product design. Just compare today’s tennis racket, road bike, or aeroplane wing to those of 30 years ago.

The complex composition of new materials imparts finely tuned performance characteristics that have to be maintained within tight tolerances. This means that analytes have to be separated from a complex matrix of concomitant material. These more difficult separations require even better chromatography, and place a real constraint on instrument‑size reduction, or throughput improvements. However, the growing use of MS/MS techniques greatly simplifies data for complex mixtures, improving specificity and certainty.

The global shortage of helium has meant that new laboratories struggle to secure helium gas cylinders, so there is a desperate need to develop GC–MS technology that is fully compatible with a hydrogen carrier—ideally with the performance levels we’ve come to expect when using helium.

There are some complications in the development of the GC–MS platform, especially if you consider tandem mass analyzers. The past decade has seen the refinement of the gas chromatograph as a platform. Improvements in flow control and rapidly responding thermocouples and heating elements have greatly increased retention time reproducibility for methods with complex temperature programmes. On the other hand, detector sensitivity has been improving by an order of magnitude every few years. There are now single quadrupole instruments available from multiple vendors with sources that are so efficient at generating and delivering ions to the mass analyzer that their sensitivity has greatly outpaced improvements in the inertness of the sample pathway, so most end users are not able to take advantage of this leap in sensitivity.

The inert sample pathway is one major challenge for the consumables vendors. Short narrow columns could be used to reduce the analyte residence time on‑column, which reduces the probability of degradation or adsorption. Faster run times are always desired, however, this raises its own issues. Column selectivity is temperature-dependent, so to preserve the separations we are used to, we would need to be capable of very fast ramp rates, and fast ramp rates require very fast and accurate electronic pressure control.

Q. What was the biggest accomplishment or news in 2019/2020 for GC or GC–MS?

We have already reached next generation GC–MS. From my point of view, the biggest recent accomplishments in GC have been focused on sample pretreatment before the GC analysis, such as thermal desorption, online analysis, and on-site sampling devices. New detection systems, such as plasma detectors, have also become more popular while many traditional GC–MS/MS applications are beginning to move towards LC–MS/MS as a result of new ionization techniques.

The latest data handling systems have also brought together GC, GC–MS, LC, and LC–MS/MS under the same software platform, making the workflow inside laboratories much more flexible and easier to operate by “generalist” chromatographers.

By far the biggest achievement in 2019/2020 was smart‑connected technology, developed originally for cutting‑edge next‑generation systems, now being extended to mainstream GC and GC–MS systems. The fact that this enabling technology is now available in market‑leading mainstream systems, across high‑end, mid‑range, and micro‑GC platforms, means it will get into the hands of far more people. This is an inflection point in terms of productivity improvement and resource deployment that will have a huge lasting impact on efficiency gains in the analytical industry. As importantly, laboratories are returning to work in split shifts to minimize on-site staff numbers during the COVID pandemic. This means expertise on-site during a single shift is unlikely to be available on all three extended shifts. Smarter instruments help trouble‑shoot faster to get up and running sooner. Remote connectivity helps connect a remote expert to the on-site instrument. These smart connected functions are invaluable as laboratories return to work in a pandemic.

Modern GC–MS and GC×GC–MS instruments allow us to gain greater insight into sample compositions than ever before. Until now, data analysis has remained a challenging prospect. The rise in untargeted “discovery-based” workflows has finally put pressure on instrument manufacturers to develop software that can tackle these huge volumes of data. New software tools are now available to extract meaningful results using all of the raw data, without resorting to hours of manual pre‑processing or complicated statistics—making discovery workflows more amenable to routine labs.

The past decade has seen several advances and accomplishments in GC and GC–MS, though the last year was fairly quiet. There aren’t any notable accomplishments in 2019/2020 for GC or GC–MS that come to mind.

 is an EMEAI Subject Matter Expert for Chromatography and Mass Spectrometry Solutions at PerkinElmer, Inc.



 is Associate Vice President, Marketing Gas Phase Separations Division, at Agilent Technologies.



 is Business Development Manager (Americas) at SepSolve Analytical Ltd.



 is a Senior Scientist in GC Solutions at Restek Corporation.

A panel discussion on the latest advances and future developments in gas chromatography mass spectrometry (GC–MS).

Trends and Developments in GC and GC–MS

In a previous Incognito, I discussed ways in which laboratory managers could improve the working conditions for analytical chemistry staff to improve their theoretical GlassDoor ratings and, most importantly, to produce an efficient and successful analytical service to the business or whomever the laboratory serves (1).

We spend a large amount of our lives at work, and now more than ever before, we demand a lot of our employers and have high expectations around working environment, company culture, connectedness to the business, health and welfare, and job satisfaction.

However, as analytical laboratory staff, we must realise that this is not a one-way street. We must give back at least as much as we receive. I’ve never seen an employee charter which didn’t include both employer and employee commitments. Beyond the “body‑shop” laboratories, where numbers of feet on the laboratory floor are the only thing that matters (and yes – these do exist), there are many organisations where one can have a truly meaningful and fulfilling career, but to find your ideal job, you need to give at least as much as you take and in most cases this involves going the extra mile in a number of key areas.

As an analytical chemist you have to realise that the number of really “sweet” job roles are few and far between, and to have the best career possible, you need to show that you have what it takes to excel in what is still a fairly crowded jobs market. Whilst your modern education and fully flexible attitude to whom you work for (or actually ‘work with’ in the modern world), will get you so far, in order to get the best jobs, you simply have to put in more effort and show a better attitude than those with whom you are competing.

The following commentary gives a bunch of suggestions of the attitudes and behaviours that I believe sets an analytical chemist apart from the crowd and is based on traits I’ve observed in a host of folks for whom I have worked for and with.

You should have a good understanding of your business, critically the aspects which are served by the analytical data that you produce. What products or services are served by your laboratory and what difference will your data make? Are you providing information for product development, if so which products and why are they better, or what new application will they support? If you are providing project support, what are the aims and objectives of the project both, of your immediate stakeholders but for the wider business? Do you provide manufacturing support, once more, what are the products and what are the critical factors in controlling the product quality and/or characteristics? Get to know the stakeholders who will use your data, and importantly how it will be used. What are their aims and objectives, what are they expecting to use your data for, what critical decisions will your data underpin? All of this information will be useful in the context of your analysis, helping you to make decisions on vital aspects of your work such as which analytes are more critical to measure to what level of sensitivity, the performance characteristics of a method you may be developing or the requirements for fast turnaround of data. Importantly, understanding the context of your client will help you to guide them on what your data might be used for, what decisions may be taken using your data and critically what decisions are not supported by the data and what are the limitations of the information you are providing. If you can get yourself an invite to Project Meetings this is a great start to help contextualise the data, but just asking to speak with your laboratory managers or the clients who use your data can be quicker and equally as informative.

Take time to understand your analyte(s) and the sample matrix, without this information it’s impossible to carry out your work with the required level of insight to produce excellent analytical data. Matrix complexity, chemistry and stability are all important when considering sample preparation, the finesses to which you will need to apply chromatographic methods, and the correct choice and optimization of instrumental parameters. What variations in matrix chemistry might you find between different products, formulations, or samples that you are testing and how will this affect the analysis? Of course the same may be said regarding your analytes, unless of course you are screening for complete unknowns. I talk to hundreds of analytical chemists who perform routine analyses on analytes whose chemical structure they do not know. How on earth can one effectively troubleshoot, let alone optimise, a method if the structure, functional group chemistry, and physico‑chemical parameters (molecular weight, solubility, stability, pKa, LogP(D), and so on) are unknown? You need to show initiative because this information may not be readily available, but find out as much as you can regarding your analyte(s) and matrix, and link these facts to your analysis.

Take great interest in the working principles of your instrument and data acquisition/analysis software. Most of us can use the basic functions, enough to get by and produce a result, but you need to do more than that. You need to understand the subtle parameters which can affect data acquisition, but which remain unchanged in most method specifications. If you “load methods” into a system and/or are locked out of changing any of the method parameters, ask your line manager for a printout of the method and try to understand each of the instrument variables, what they influence, and why the particular values for each have been selected. You need to understand what the equipment is capable of and what it is not, as this will directly affect your assessment of data quality. You need to get to the point where you can spot an instrument that is underperforming or where equipment can perform better than it is currently configured to do – and can make suggestions for possible improvements. My oft quoted example is, if you use a mass spectrometric detector, have you ever manually tuned that instrument to see if you can do better than the “autotune” function using either the embedded tune compound for GC–MS or by infusing a test compound in LC–MS, and then adjusting parameters to see what affect they have on detector performance? If not – ask someone to show you how this might be done, if indeed there is anyone who knows. If there isn’t anyone with this level of knowledge, ask for some vendor training.

The same is true of software, and you should be aiming to understand not just those variables that you typically input, but the subtle software settings that can often make a big difference to the quality or speed of data analysis. Become familiar with integration algorithm settings, take an interest in the calibration settings, the system suitability specifications, and quality control checks. Get yourself into a position where you can reproduce the result generated by the data system by working through the calculation of the result from the raw peak areas generated by the data system. This is a salutary exercise that is often much more difficult than it might sound.

Learn what constitutes good and bad data. Not just whether the results pass or fail, but what you should look for in terms of the quality of your chromatographic output. Peak shapes, baselines stability and appearance, peak resolution, and peak efficiency are all important indicators of the quality of your instrumental output and you should learn, over time, to spot even the most subtle signs that all is not as it should be. This will then lead you onto understanding some of the fundamentals of chromatographic science, the underpinning theory behind the separations and detection you are tasked to carry out. Having a deeper understanding of the basic theory will, I promise you, improve your work and the enjoyment you derive from your producing that work. If you don’t know what plate count is, how it can affect the appearance of your chromatogram, and what plate numbers can be expected from the separation you are undertaking, then this paragraph applies directly to you, and this is one example from a myriad that I can quote here.

Run towards problems and not away from them. Immerse yourself in troubleshooting if you are able. If your metrology department or external service provider does all of the equipment preventative and reactive maintenance, spend time with those engineers and learn as much as you can from them. Becoming involved with troubleshooting discussions on chromatograms, methods and data, is invaluable for you to gain a deeper understanding of chromatographic science, what goes wrong and why it goes wrong. You will spend a lifetime learning these things, but the more you know, the more links you can make between symptoms and causes and the more efficiently you will be able to diagnose problems and fix them. It is hugely rewarding to able to fix problems which help to overcome potential crises with the speed or quality of information provision from your laboratory.

Academic journals, industry publications and vendor publications are all rich sources of information and as such you should be selecting articles or applications which are pertinent to your work and really striving to understand the information and its application to your own particular analysis. You can then progress to topics which are outside your current applications or instrument techniques, to the latest thinking on application developments and the broader literature. Your reading will directly affect the effectiveness of your work, again I personally guarantee this to be true. The fact that you are reading this Incognito instalment bodes well in this respect, and I see a bright future for you dear reader! If someone uses a term or presents information which you do not understand, then ask for an explanation. One cannot know everything about everything, and you should expect to learn new facts, concepts, and ideas throughout your career and embrace that this is a fundamental truth. Crucially you need to then digest this new information and think about how it might apply to your work or how you might use this knowledge to improve your daily practice. To a relatively new practitioner, the language of analytical science can be foreign and almost intractable, but persevere, for like any new language, skill will come with practice. It’s not a sign of weakness to ask when you don’t understand, only laziness NOT to ask, and your thirst for broader and deeper understanding should be voracious. Reading widely will also help to improve your scientific writing skills, a topic that many of us find difficult. There is a certain style to scientific writing and even more subtleties to writing about analytical science. Children studying their native language and literature are told to read widely to improve their writing style, the same is just as true for the language of science.

Attend every relevant training event, external meeting, conference and exhibition that you can. Critically, make sure that you make the effort to come away with new skills or knowledge and make a point of summarising and sharing these (either formally or informally) with your colleagues. Again, a broader and deeper understanding of all aspects of chromatographic science and your application of that science will improve your effectiveness and enjoyment of the work you do. From every event, make a bullet point list of everything that you wish to bring into your practice or new ideas or approaches that may bring improvements, and tick these off your lists as you address them. Not all will be successful, but your aim should be to pay back the business for the extra learning and development that have been afforded to you.

Push yourself out of your comfort zone when it comes to writing and presenting. Project review reports, new instrument evaluations, protocols, SOP’s, analytical reports, troubleshooting reports, and laboratory investigations are but a few examples of where you can practice your writing skills. This will probably involve some discretionary effort on your part, but this is the price of becoming an exceptional analytical scientist, just as it is with any career. Producing and delivering presentations is something that strikes fear into the heart of many a good scientist, but writing a presentation and building a slide deck is often linked with better understanding of the scientific topics contained within and the presentation itself will help you to distil the critical aspects of this science even further, which, in turn, will hone your analytical understanding and scientific communication skills.

Honestly, if you turn up to work to push buttons and produce numbers, that isn’t a problem, so long as someone else is making sure the numbers are meaningful. However, if this is the case, please do not complain when others, who show more interest in the topics outlined above, get promoted ahead of you or get all of the interesting jobs. If you do find satisfaction in operating laboratory equipment and this is what you would like to do for your career, this is genuinely praiseworthy, but again, please make sure that you are the best equipment operator you can be, and to do that, you will need to pay attention to at least some of what I’ve written above.

Of course, for employers reading this article and realising that few, if any, opportunities described above are afforded to your employees – I refer you to my previous article “How would your Company do on Glassdoor?” (1).

The writer Elbert Hubbard once remarked, “Initiative is doing the right things without being told”, ask yourself which right things you will be doing in the laboratory today?

(12), 19–21 (2019). www.chromatographyonline.com/view/how-does-your-laboratory-measure-glassdoor

Get set for greater success in your career as an analytical chemist, with Incognito’s practical suggestions that will make you stand out from the crowd. These tips for excellence will enlighten employees and employers alike.

The Excellent Analyst

As a result of the unique nature of per- and polyfluorinated alkyl substances (PFAS) and their emerging health concerns, testing methods have evolved to be more efficient and solid-phase extraction (SPE) has become an essential clean-up step in the PFAS workflow. Since the original promulgation of regulated methods, new compounds have been identified and the investigation of more diverse matrices have made it increasingly more difficult to extract and analyze PFAS. This article explores the role of SPE sorbents for analyte recovery rates and method accuracy to develop clean samples for analysis and to reach lower limits of detection.

Per- and polyfluorinated alkyl substances (PFAS) are potentially harmful compounds that have been introduced to environmental, food, and biological samples as a consequence of their widespread commercial use over the past 50 years. Analysis of these compounds has been historically difficult because of their overwhelming prevalence, multiplicity of chemical analogues, and closely related molecular structures. Consequently, the need for more efficient analysis and extraction of PFAS has significantly grown, with the need to adopt methods for diverse sample types as well as to account for the proliferation of PFAS structure.

As newer methods are adopted there has been a strong focus on sample preparation method that act as the vital part of the extraction and clean‑up portion of the PFAS workflow. The original United States Environmental Protection Agency (EPA) 537 Methods were limited to a list of 14 analytes and the sample matrix was restricted to drinking water. This simplicity made the methods relatively straightforward with regards to solid-phase extraction (SPE) and LC–MS/MS analysis. However, with the expanding list of PFAS compounds and matrix diversity, the methodology has evolved and SPE sorbent chemistry has become much more important for achieving the accurate analysis of PFAS in environmental samples.

SPE is one of the most versatile modes of sample preparation, employing a unique combination of sorbent chemistry and elution conditions to bind, clean‑up, and release analytes in simple, sequential steps. When done effectively, SPE can achieve three essential goals in an extraction: clean‑up the matrix, concentrate the sample, and provide a solvent-switching mechanism to a more compatible mobile phase that is more compatible with mass spectrometry (MS) analysis. Consequently, many laboratories choose SPE over less complicated, but less versatile methods because even though the method development process may be longer, SPE results in a cleaner extract that is easier to process by LC–MS/MS.

There are diverse sorbent options available for SPE, both silica-based and polymer-based, so one first needs to understand why certain SPE sorbents are selected for certain PFAS extractions. To begin the sorbent selection process, the characteristics of the sample matrix first need to be determined. For PFAS testing this could be drinking water, wastewater, soil, sediment, food samples, or even tissue, or whole blood. The next step in the SPE sorbent selection is to consider the analytes of interest, in this case PFAS. Once the sample matrix and target analytes are considered, this will determine the SPE approach that is the best fit for the analysis.

The common extraction/elution steps for a reversed‑phase sorbent method are presented in Figure 1. While seemingly straightforward, many issues can arise in SPE from both sorbent selection and wash/elute solvent selection. Considering that PFAS consist of both long and shorter chain compounds of varying hydrophobicity, care must be taken in the wash and elution steps to obtain a balance between ultimate sample cleanliness and analyte retention on the sorbent. Too strong a wash will result in low analyte recovery, but too weak a wash will result in insufficient sample clean‑up, potentially impacting the MS analysis. Since the regulated methods present a final, optimized set of conditions and do not discuss the SPE optimization process, the reader must rely on method development applications or white papers for more detailed treatment of the process, which can be found at vendor or publication websites.

Since sorbent selection for SPE is derived from the combination of analytes and the sample matrix, the official EPA Methods communicate specific sorbent types based on the specific analyte list. EPA developed their first official PFAS Method (EPA Method 537) (1) specifically for drinking water to support the third Unregulated Contaminant Monitoring Rule (UCMR 3) (2). It consisted of 14 PFAS compounds with a focus on perfluorooctanesulfonic acid (PFOS) and perfluorooctanoic acid (PFOA) which had the highest historical usage. The original EPA 537 analytes are also included in the EPA 537.1 update along with four additional shorter-chain PFAS compounds (the so-called 

 compounds) that had been subsequently introduced into manufacturing and now require analysis. Since all the compounds in the list hold the generally similar hydrophobic analyte characteristics of long chain alkyl substances, Method 537.1 continued to recommend a polystyrene‑divinylbenzene (PS‑DVB) for the extraction step. PS‑DVB is a polymeric sorbent that offers hydrophobic selectivity for reversed-phase application and works well to extract long chain and the four additional shorter chain PFAS with high recovery. Figure 2 displays analytical results for the PS-DVB SPE method used in EPA Method 537.1 showing how both the long chain and shorter chains PFAS are adequately resolved by LC–MS/MS analysis with excellent retention.

A more recently-released method (EPA Method 533) was developed to complement the original method for PFAS analysis with an expanded list of 25 analytes with a greater diversity of chemical characteristics which offers a more complete solution for both the long chain and shorter chain PFAS compounds. However, the originally recommended PS‑DVB SPE sorbent may result in low analyte recoveries because some newly added compounds, such as pentafluorobenzoic acid (PFBA) and perfluoropentanoic acid (PFPeA), are too polar to be retained on the reversed‑phase SPE sorbent. For the 533 analyte list, a polymeric weak anion-exchange (WAX) sorbent was stipulated, having affinity for both the original, hydrophobic analytes and the new more polar/acidic PFAS analytes which are retained by an anion-exchange mechanism. In Table 1, a basic comparison of the two EPA Methods is presented. Table 2 presents analytical data for Method 533 showing high precision and accuracy for all 25 analytes, including PFBA and PFPeA.

Complex sample matrices such as oils, sediments, treatment sludges, and biota (fish, benthos, etc.) are gaining greater attention as scientists seek to better understand the transport and fate of PFAS in the environment. Per the US Department of Defense (DOD) guidelines (DOD QSM 5.1/5.3), which outline testing of PFAS from non-drinking water sources, it states that weak anion-exchange (WAX) SPE sorbent in combination with graphitized carbon black (GCB) material is specified for added cleanliness. Traditionally there have been two ways to perform this procedure, both of which are time consuming and sometimes yield inaccurate results owing to their complex SPE processing procedures. One method employs a single SPE cartridge to extract the analytes followed by another SPE cartridge filled with GCB material to remove additional contaminates from these especially dirty matrices. A second method uses SPE cartridge sorption and the SPE eluate followed by GCB treatment in a dispersive mode (dSPE). For both approaches, significant time is required for the clean‑up and the multiple steps can present an opportunity of analyte loss and imprecision.

However, a new technology was recently released, that offers improved precision and accuracy by combining both SPE sorbents into a single tube. By combining both WAX and GCB sorbents into a single tube in a stacked manner, waste and time can be reduced while also improving accuracy. In addition, this single tube method is more economical owing to more rapid sample processing and reduced material cost (for example, one tube instead of two).

Table 3 presents data for the stacked cartridge solution. These data demonstrate acceptable method performance and data acceptability of all 32 analytes within method recovery limits. With an average analyte recovery of 98.8% and mean recovery of 99.0%, this demonstrates that the stacked SPE cartridge is “fit for purpose” in the performance DOD QSM 5.1/5.3.

In addition to their presence in traditional environmental samples, PFAS are also prevalent in food products due to environmental impacts, thereby heightening concerns about human exposure and health effects. SPE sorbent selection is further complicated by this additional increase in matric diversity and complexity. However, Figure 3 displays a good starting point for evaluating the types of retention mechanisms that could be used for the extraction step. In this case, the sample matrix is extremely important to determine the optimum SPE retention mechanism. From there, specific SPE phases would be selected based on the PFAS analytes of interest. Most vendors offer additional tools to help determine the starting SPE sorbent and recommended protocol to begin with. In particular, the QuEChERS clean‑up procedure has been shown to be applicable for fatty food matrices (milk, cheese, fish, and so on) and for biota.

The process of defining PFAS extraction and purification conditions may seem extremely complex owing to the multiplicity of PFAS and their presence in diverse matrices. However, we have shown that breaking down specific methods according to the chemical characteristics of the target analyte list and the nature of the sample matrix can be very useful in defining optimal SPE sorbent selection and operating conditions. This then serves as the starting point to define the overall PFAS workflow. Good method accuracy and precision start with effective sample preparation, and SPE has been shown to provide a reliable foundation for PFAS method performance. As new SPE technologies are developed further, gains in analytical method performance can be expected, as well as commensurate gains in sample throughput and laboratory economics.

J.A. Shoemaker, P. Grimmett, and B. Boutin, 

Determination of Selected Perfluorinated Alkyl Acids in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry (LC/MS/MS)

 (U.S. Environmental Protection Agency, Washington, D.C., 2008).

Contaminant Candidate List 3 (CCL 3) https://www.epa.gov/ccl/contaminant-candidate-list-3-ccl-3

Method 537.1: Determination of Selected Per- and Polyfluorinated Alkyl Substances in Drinking Water by Solid Phase Extraction and Liquid Chromatography/Tandem Mass Spectrometry

 (LC/MS/MS) (U.S. Environmental Protection Agency, Office of Research and Development, National Center for Environmental Assessment, Washington, D.C., 2018).

D. Kennedy, S. Lodge, and A. Pierri, https://phenomenex.blob.core.windows.net/documents/e4265f51-d6db-42ac-9ee6-d8fad055b844.pdf, accessed on Sep. 14, 2020.

A. Patterson, C. Neslund, R. Brown, S. Lodge, D. Kennedy, and B. Marshall, https://phenomenex.blob.core.windows.net/documents/ba582f2f-4927-4408-aace-4ecfff1a51c2.pdf, accessed on Sep. 14, 2020.

A. Pierri and S. Lomas, https://phenomenex.blob.core.windows.net/documents/234361ad-5022-4cad-bb0a-5514059a1ba5.pdf, accessed on Sep. 14, 2020.

S. Estil, E. Nelson, and S. Krepich, https://phenomenex.blob.core.windows.net/documents/2c9677ab-4ca8-450e-a134-6de2fc54a92a.pdf, accessed on Sep. 14, 2020.

https://www.epa.gov/pfas/epa-pfas-drinking-water-laboratory-methods, accessed on Sep. 14, 2020.

https://www.epa.gov/ground-water-and-drinking-water/drinking-water-health-advisories-pfoa-and-pfos, accessed on Sep. 14, 2020.

 graduated from Vanguard University of Southern California (California, USA) with a B.S. in biology and a minor in chemistry. She now works as a Product Marketing Manager for sample preparation products at Phenomenex, Inc. located in Torrance, California, USA.

This article explores the role of SPE sorbents for analyte recovery rates and method accuracy to develop clean samples for analysis and to reach lower limits of detection.

Advances in Solid-Phase Extraction to Improve the Analysis of Per- and Poly-fluorinated Alkyl Substances

Rachael Szafnauer received an M.Sci in forensic science from the University of South Wales, UK, where her final‑year project focused on fingerprinting emerging psychoactive substances using advanced techniques such as GC×GC–TOF MS, in collaboration with Markes International. She later took up the role of thermal desorption product specialist at Markes, providing technical and application support to the commercial team, before taking on her current role at the start of this year, specialising in the development of applications using extraction and enrichment techniques.


Elinor Hughes obtained her B.Sc. in chemistry and Ph.D. in organic chemistry at Bangor University, UK. After working for a chemical manufacturing company for three years, she moved to the Royal Society of Chemistry where she worked in journals publishing for six years and on Chemistry World magazine for four years. This was followed by five years as a freelance copyeditor and science writer. Her current role is technical copywriter at Markes International.

High-capacity sorptive extraction is a sampling technique that involves using a probe to extract volatile and semi-volatile organic compounds (VOCs and SVOCs) from samples for analysis by thermal desorption–gas chromatography–mass spectrometry (TD–GC–MS). Samples can be taken from the headspace of a liquid or a solid, or by immersing the probe in the liquid. This study demonstrates how the technique can improve on traditional methods in the analysis of VOCs that contribute to the aroma and flavour of a breakfast cereal and in identifying other compounds of interest, such as food additives, contaminants, and potentially toxic compounds at trace levels.

Within the food industry, there is an increasing need to monitor product quality and safety to understand flavour composition and product contamination, and to determine how these relate to both consumer satisfaction and effects on human health. This analysis requires a detailed understanding of individual components of a product, but conventional approaches to sample preparation and gas chromatography–mass spectrometry
(GC–MS) analysis can struggle to provide the necessary level of sensitivity.

Traditionally, solid-phase microextraction (SPME)—in which a fibre coated with an extracting phase (known as the sorptive phase)—has been used to sample volatile organic compounds (VOCs) from foods and beverages. SPME offers simple, solventless sampling and is easily automated for high‑throughput applications. However, it is limited by the amount of sorptive phase (to ~0.5 µL) and the fragility of the fibre (1). More recently, thicker sorptive films and stir bars with a sorptive phase have been used to enhance sensitivity; however, the latter approach is limited in scope due to the manual interactions required by the user (2).

High‑capacity sorptive extraction can overcome these issues. Firstly, the use of strong, metal‑core probes supporting a higher amount of sorptive phase (~65 µL) means they are less prone to damage and provide a more robust extraction technique with improved sensitivity (3). The technique can also be fully automated, from sample extraction and post‑sampling probe washing and drying through to desorption and GC injection. It is also possible to preconcentrate multiple extractions onto a single focusing trap prior to GC analysis—a process known as multi‑step enrichment (MSE) (Figure 1). This increases the extraction efficiency of the technique, which leads to a higher column loading of analytes, enhancing the sensitivity and number of compounds detected.

In this study, the volatile organic chemical profile of a breakfast cereal was analysed using high‑capacity sorptive extraction first and then combining it with MSE. This enabled a broad range of VOCs contributing to the flavour and aroma of the product to be identified. Additionally, food contaminants, potentially from the product’s packaging and the original cereal crop, were detected.

Sample Preparation and Extraction: A store-bought breakfast cereal (1 g) was homogenised prior to addition of NaCl (2.5 g) and distilled water (10 mL). Headspace extraction of VOCs was performed on the Centri extraction and enrichment platform (Markes International Ltd) using two modes: (a) HiSorb, a single-vial extraction for analysis and (b) HiSorb with MSE, loading four extractions from different, replicate sample vials to the trap prior to analysis. HiSorb probe: Short-length (48 mm) stainless steel (Markes International Ltd, part no. H1-XXABC); Incubation: 75 °C (20 min); Probe desorption: 250 °C (10 min); Flow path: 180 °C; Focusing trap: Materials Emissions (U-T12ME-2S) (Markes International Ltd); Purge flow: 50 mL/min (1 min); Trap low: 20 °C; Trap high: 280 °C (5 min); Heating rate: MAX (>100 °C/s); Split flow: 5 mL/min.

Gas Chromatography (GC): Instrument: Agilent 7890 GC system (Agilent Technologies); Column type: TG‑624, 30 m × 0.25 mm × 1.4‑μm (Thermo Fisher); Column flow: Helium, 1.5 mL/min (constant flow); Oven program: 50 °C (5 min), 15 °C/min to 240 °C (10 min).

Mass Spectrometry (MS): Instrument: BenchTOF-Select mass spectrometer (SepSolve Analytical); Mass range: 

ChromSpace GC×GC software (SepSolve Analytical) was used for full instrument control and data processing.

Volatile and Semi-Volatile Organic Compounds (VOC/SVOC) Profile Analysis: Cereal samples were extracted using sorptive extraction probes, initially for a single-vial analysis, followed by MSE, where four headspace extractions were taken from separate vials for one GC analysis. Figure 2 shows the total ion chromatogram (TIC) for both the enriched (upper black trace) and single (lower inverted red trace) extractions. It is clear that an enhancement in sensitivity is achieved across the entire sample profile when using enrichment compared to a single extraction, with no compromise in peak symmetry or resolution. MSE provided a more comprehensive sample profile so the results using this technique are discussed in the following sections.

In total, 150 VOC/SVOC compounds were detected by MSE. The identification of compounds that had a peak area >1% of the TIC and with a NIST match factor >750 are shown in Table 1, with odour descriptors (where available) and odour threshold values (the concentration at which an aroma or taste can be detected).

In a sample this complex with significant chromatographic co‑elutions (where two [or more] compounds do not separate chromatographically so they are difficult to see), spectral deconvolution is critical for a more confident identification of VOCs present. Deconvolution is a data processing technique that can be applied to complex elution profiles. It was carried out in this study using data analysis software with resulting spectra compared to compounds in the NIST 2017/EPA/NIH mass spectral library (6). The inset in Figure 2 shows an example of this. In this instance, the deconvolved peaks were identified as the SVOCs dibutyl phthalate (DBP, a plasticiser) and tris(2-chloroisopropyl) phosphate (Amgard TMCP, a flame retardant).

Other compounds of interest from a food toxicity/contamination perspective (text labelling in Figure 2) were also detected and will be discussed in more detail later.

The range of VOC/SVOC compounds identified is wide, as demonstrated in Figure 3. The bar chart shows the distribution of the number of components for each compound class. The profile was dominated by aldehydes, alkanes, alcohols, heterocyclics, and aromatics. Within these classes, the most abundant compounds were hexanal (green, grassy) at 5.6% (of the TIC), piperonal (cherry, sweet) at 5.5% (of the TIC), and vanillin (sweet vanilla) at 5.3% (of the TIC). During the production (heating) process of the cereal, Maillard reactions (chemical reactions between amino acids and reducing sugars) occur and therefore a large amount of these compounds would be expected. Several compounds that are known to give an unpleasant or off-odour were also detected, for example, four thiols/organo-sulfurs and three phenols (Figure 3), albeit at relatively low levels.

Principal component analyses for VOCs and SVOCs are important for characterizing the aroma and flavour profiles of food products, and the odour threshold value (OTV) is an associated parameter. Therefore, detection and identification of trace VOCs can be significant, particularly for compounds with medium and low OTVs or for problematic compounds (such as malodours) with low values, so that subsequent remedial action can be taken if necessary.

MSE provides a mechanism to increase the amount of each compound introduced to the GC, thus increasing the number of compounds detected, extending down to trace-level components. As representative examples, compounds such as dihydro‑5‑pentyl-2(3H)-furanone (γ-nonalactone), anethole, and γ-terpinene were detected in the single extraction but at very low levels where their spectral quality was not sufficient for a good library match. Figure 4 demonstrates how MSE enabled a more confident identification for these compounds, and this is indicated in the NIST values shown in parentheses in Table 2.

Other components, such as eucalyptol, phenyl ethyl alcohol, and α-farnesene were only detected in the enriched sample, meaning they could have been missed had only a single extraction been used for analysis (Figure 5). Eucalyptol is an important component in the sample with a relatively low OTV (12 ppb), imparting a herbal or camphor aroma to the product. These compounds are listed in Table 2. The NIST values represent the enriched sample with comparison to the single point extraction in parenthesis when a partial response was observed.

Additives and Compounds with Potential Toxicity

Along with VOCs related to odour and taste, several additional compounds were identified in the breakfast cereal (Figure 2, Table 3). These include the antioxidants butylated hydroxytoluene and 2,6‑di‑tert‑butylphenol, known to be added to food to prevent spoilage, and several compounds that potentially originate from the food packaging as contamination: styrene, two phthalates and two cyclic lactams. Interestingly, compounds that are usually associated with combustion were also detected in this sample (benzene, toluene, ethylbenzene, and xylene), with the possibility that these are present due to contamination of the original cereal crop.

Furthermore, compounds present on the US EPA Toxic Substances Control Act (TSCA) list (7) were tentatively identified (Figure 2, Table 3), such as butyphos (tributylphospine oxide), a herbicide, Amgard TMCP (tris(2‑chloroisopropyl) phosphate), a flame retardant, and naphthalene, a PAH. Although this analysis was only qualitative, so no indication of the concentration can be inferred from the data, the detection and tentative identification of these compounds demonstrates that high‑capacity sorptive extraction can provide the ability to extract and analyse a wide range of compounds in addition to the main flavour and odour‑active compounds of interest.

In this study, we have demonstrated the use of a fully automated high‑capacity sorptive extraction technique for profiling the VOCs present in the headspace of a breakfast cereal using preconcentration with a single‑vial extraction and multiple extractions. A wide range of compounds pertaining to taste and odour were found. Several components were found only in the enriched sample, demonstrating how multi‑step enrichment provides a more comprehensive extraction, which leads to a more accurate VOC profile of a food sample. The fast MS acquisition combined with data processing further enhanced the identification of compounds, enabling co‑eluting peaks in the complex profiles to be distinguished into individual analyte peaks. Moreover, the ability to discover compounds present in the sample that either contribute to off‑odours, have migrated from the packaging, or are contaminants from the original food commodity is important because they have potential toxicity and could affect human health. This breadth of compounds discovered demonstrates the enhanced capability of the extraction methodology. Lastly, the automated extraction and enrichment process means that no human interaction is required from sample extraction through to GC injection, allowing faster sample throughput. This ensures high productivity is achieved in industrial laboratories such as contract service or food research.

N.-E. Song, J.-Y. Lee, Y.-Y. Lee, J.-D. Park, and H.W. Jang, 

U. Telgheder, N. Bader, and N. Alshelmani, Asian J. Nanosci. Mater. 1(2), 56–62 (2018).

https://www.markes.com/Products/Sampling-accessories/HiSorb-sorptive-extraction.aspx

The Good Scents Company Information System, www.thegoodscentscompany.com, search facility accessed on Sep. 11, 2020.

Odour and Flavour Detection Thresholds in Water (ppb) – Leffingwell & Associates, http://www.leffingwell.com/odorthre.htm, accessed on Sep. 11, 2020.

https://sciencesolutions.wiley.com/solutions/technique/lc-ms/nist-epa-nih-ms-ms-mass-spectral-library-2017/

United States Environment Protection Agency, www.epa.gov/chemicals-under-tsca , accessed on Sep. 11, 2020.

 received an M.Sci in forensic science from the University of South Wales, UK, where her final‑year project focused on fingerprinting emerging psychoactive substances using advanced techniques such as GC×GC–TOF MS, in collaboration with Markes International. She later took up the role of thermal desorption product specialist at Markes, providing technical and application support to the commercial team, before taking on her current role at the start of this year, specialising in the development of applications using extraction and enrichment techniques.

obtained her B.Sc. in chemistry and Ph.D. in organic chemistry at Bangor University, UK. After working for a chemical manufacturing company for three years, she moved to the Royal Society of Chemistry where she worked in journals publishing for six years and on Chemistry World magazine for four years. This was followed by five years as a freelance copyeditor and science writer. Her current role is technical copywriter at Markes International.

This study demonstrates how the technique can improve on traditional methods in the analysis of VOCs that contribute to the aroma and flavour of a breakfast cereal and in identifying other compounds of interest, such as food additives, contaminants, and potentially toxic compounds at trace levels.

Improved Aroma Profiling of Foods by High-Capacity Sorptive Extraction

As one would expect of any technology, each passing year shows some incremental advantage in chromatography. The realization of these advantages comes through an incredible amount of carefully thought‑out and conscientious effort. Some areas where we consistently see incremental improvement in chromatography are:

We are now at a time, however, when our focus should no longer concern itself with the incremental, and instead focus on a big idea that will alter the course of chromatography forever. This big idea is, without a doubt: miniaturization.

The trend towards miniaturization is visible in many areas of the wider world. Items such as our wristwatches and cellular phones take up newly developed technology, allowing them to be trimmed down without sacrificing qualities consumers have come to expect, and subsequently demand. Chromatography systems, accessories, and workflows are all following suit; this has taken some years to build, but is now advancing rapidly. Large and small companies have joined in this effort. While common themes are evolving, there is no shortage of different approaches to solving the multitude of problems created, as well as opportunities afforded by, miniaturization.

To miniaturize chromatography, the engineering and fabrication feats are tremendous. For example, as sample pathways, tubing, and systems narrow and shrink, so do the design tolerances. To address this challenge, many companies are returning or keeping manufacturing in their home countries: Instruments are built by hand in high-end facilities by qualified engineers—a job that is typically shipped out to overseas partners for the majority of contemporary chromatographic instruments.

Another big obstacle is the bureaucratic administration of large agencies, such as the Food and Drug Administration (FDA) and Environmental Protection Agency (EPA), governing the most productive analytical laboratories in the USA. These organizations are, by nature, cautious, and often seemingly resistant to “course correction”. Novel instruments are less likely to serve these controlled environments, which boast the highest density of instrumentation—thus slowing innovation.

All the obstacles in the world, however, cannot stop innovation, but merely slow its inevitable march. Some advantages are so evident and incredible that they overcome even the most vigorous resistance. One such advantage of miniaturized chromatography—as simple as it is powerful—is that as systems reach a tenable size for overnight shipment, the need for a traditional and cumbersome service network naturally falls away. This is because, if you need instrument repair, you can quickly receive a stand-in instrument to use while you send out your broken unit for repair, without needing to have a service engineer visit your site. This change has the potential to halve the cost of running instrumentation in the field.

Another game-changing advantage of miniaturization is that smaller channels and sample pathways dramatically decrease the need for gasses, solvents, and power requirements. This feature further allows a more portable or mobile paradigm to evolve, while lowering costs and waste.

While there isn’t enough space here to go through all the fantastic attempts to miniaturize chromatography instruments, I would like to highlight a couple of my favourite approaches for your consideration. First, I need to state that my opinion in no way reflects on my employer, this publication, nor any group to which I belong.

A favourite of mine is the approach being taken by Axcend, which offers the most portable gradient liquid chromatography (LC) system the world has yet seen. Their instrument’s tool-less design, rechargeable battery, and light weight make it compatible with almost any field application.

Another excellent offering in this field is the miniaturized gas chromatography (GC) instrument made by Lucidity. This elegant solution to an overcrowded benchtop sits on roughly a third of the space used by a traditional kit while not sacrificing any meaningful performance. Set up, run, and swap columns and consumables like a pro, from your first day. They don’t lock you into any consumables and offer the best of consumer-driven business practices that you have come to expect from other areas of life.

The best of our companies operate by standing in their customers’ shoes, solving problems as if they were their own. Innovation rooted in holistic long-term problem-solving that lovingly draws from the learnings of the previous step inspires enthusiasm for advancement from the greater community—one in which I am thrilled to be taking my part.

This blog is a collaboration between LCGC and the American Chemical Society Analytical Division Subdivision on Chromatography and Separations Chemistry.

 began his career as an analytical chemist in the pharmaceutical industry. Inspired by his long-standing love of science and natural ease with sales and marketing, he is currently working to seek strategic business solutions in the chromatography field. He works for Restek and volunteers his time to a wide variety of non‑profit organizations within the chromatography community. Edelman serves as the treasurer of the ACS SCSC, in addition to serving as Chair of the Organizing Committee for the ISCC/GC×GC 2021 conference, Executive Committee Person at the Chromatography Forum of Delaware Valley, USA, president emeritus of the Washington Chromatography Forum, and founder and president of the Separation Community Mixer.

In any given community, on rare occasions, leaders converge on a big idea. The development of such an idea alters the course of the community, in a way that is meaningful if it is lasting. It is my belief that the collective chromatography community is currently converging on a big idea.

Miniaturized Chromatography—The Next Big Idea

An analysis method for influenza virus particles has been developed using size-exclusion chromatography (SEC) which provides complimentary biopharmaceutical data for use during vaccine production and approval (1).

Vaccination is the most effective form of influenza control, preventing widescale outbreaks and pandemics from emerging. Various manufacturers produce influenza vaccines utilizing inactivated whole virus particles to illicit an immune response in the recipient via the surface antigens present on the viruses. Primarily these are Hemagglutinin (HA) and neuraminidase (N) with 17 different HA and 10 different neuraminidases being identified. As such, the amount of HA in any produced vaccine is crucial to the effectiveness and subsequent release of a vaccine for use with various guidelines existing to ensure enough HA antigen is present.

Currently, HA quantification mostly relies on two methods: the single radial immunodiffusion (SRID) assay and the HA assay. SRID is considered the gold standard and is based on antigen binding, whereas HA assays use the hemagglutination of erythrocytes. Despite its history, widespread acceptance, and various uses, the HA assay has a number of drawbacks such as the lack of standardization, its discrete format, deviations due to erythrocyte aging (2), secondary interactions of pH, buffer ions (3), and other compounds in complex virus samples. These drawbacks have become particularly relevant in recent years as authoritative bodies have sought an enhanced understanding and control of the vaccine production process with investigation of size, content, and immunogenicity of aggregates in the drug product or substance recommended. As such, numerous techniques and methods have been published offering solutions.

One such publication focused on analytical size-exclusion chromatography (SEC), a non-destructive technique that has been used for decades to analyze the aggregate and fragment content of therapeutic proteins (4). Researchers developed a robust method that handles different buffer systems, ionic strength, and additive concentrations well. Requiring the addition of 200-mM arginine or sodium chloride to obtain complete virus particle recovery. The results are confirmed by dynamic light scattering (DLS), and the universal applicability of the method was demonstrated with three different influenza virus samples, including the pandemic H1N1 vaccine strain 5258 which is an industrially-produced pandemic vaccine strain. The method adds valuable data regarding the size distribution of influenza virus samples to the commonly- used HA assay for the quantification of influenza viruses, and can potentially be used to adhere to ever stricter guidelines from biopharmaceutical regulatory bodies.

et al., J. Liq. Chromatogr. Relat. Technol. 

An analysis method for influenza virus particles has been developed using SEC which provides complimentary biopharmaceutical data for use during vaccine production and approval.

Influenza Virus Particle Analysis Using SEC

The natural speciation of metals in environmental matrices can be easily disrupted by chelators which form soluble complexes with metals. Unfortunately, the detection of such complexes during their formation in environmental matrices has remained challenging, largely because of the difficulty in obtaining the precise inherent nature of metal-chelator complexes using routine techniques. As such researchers have developed a rapid and sensitive technique for the speciation analysis of complexes of nickel, lead, cobalt, iron, and calcium, as well as two aminopolycarboxylate chelator variants, EDTA (ethylenediaminetetraacetic acid) and EDDS (ethylenediamine-N,N’-disuccinic acid). Sample preparation consisted of a simple dilution, the speciation analysis was performed using ultra-performance liquid chromatography-quadrupole/time-of-flight mass spectrometry (UPLC-Q-TOF–MS), and separation was achieved using hydrophilic interaction liquid chromatography (HILIC) (1). The effect of various operating parameters on analytes such as mobile‑phase composition, buffer concentrations and pH, sample diluents, sample injection volume, and column temperature on the peak shape and sensitivity were systematically optimized. These steps resulted in a rapid and dependable method of speciation analysis and simultaneous detection of metal-chelator complexes from environmental samples.

Researchers have developed a rapid and sensitive technique for the speciation analysis of complexes of nickel, lead, cobalt, iron, and calcium, as well as two aminopolycarboxylate chelator variants, EDTA and EDDS.