The Importance of Rapidly Accessing Reliable Analytical Consumables

Seventy-three percent of analytical lab managers report that maintenance/downtime is a top challenge for them. This blog provides an overview of some real-world issues and examples contributing to analytical downtime and how these can be remedied. This includes issues associated with the buildup of particulates in high performance liquid chromatography (HPLC) fluidics, blocked syringes, and contaminated gases used in mass spectrometry.

Many years ago, I worked as an application specialist in the field; my role was to help clients with developing, optimizing, and troubleshooting chromatographic methods, specifically for high performance liquid chromatography (HPLC). On one occasion, I was sent into a biotech company whose focus was manufacturing biological therapeutics. The company had recently noticed that they were observing a possible new impurity or degradation, due to an erroneous peak appearing on their size exclusion chromatograms. This was a serious issue, as it was risking a costly halt in the manufacturing process. Furthermore, this new peak was also posing a concern over the active pharmaceutical ingredient (API) safety profile. Therefore, it was imperative that the cause be identified and a solution rapidly implemented.

What was confusing was that the erroneous peak was appearing from new columns and not on older columns. However, having fully evaluated the issue, the root cause of the problem was not strictly column-related (such as a void forming at the front of the column), but was due to a partial blockage of the column inlet frit by particulates accumulating from the fluidics. This then disrupted the shape of the separated bands exiting the column, leading to an erroneous peak artifact “resolving” from the main product peak. It was just coincidental that the problem was seen with the newer columns.

Unwanted particulates in fluidics can be a major headache for analysts. Not only do they cause issues with the quality of the results, but they can also increase wear of instruments, leading to more frequent breakdowns. Particulates originate from a variety of sources, such as unfiltered and aging solvents, insoluble components in samples, as well as wear on seals.

It is not just particulates that are a cause of breakdowns, many other factors need to be considered too. As a result, the need for good instrument maintenance and strict adherence to lab standard operating procedures (SOPs) is critical. Moreover, timely access to good-quality consumables and parts is equally as important to prevent costly instrument downtime and maintain high-quality analytical results. For example, using high-quality syringes helps to ensure repeat and accurate injection volumes. This is something I know only too well. When I was an undergraduate back in the 1990s, I underwent a summer research project, measuring gas produced by cyanobacteria. An important part of my results was deemed unusable as this was traced back to a blocked gas chromatography (GC) syringe!

The use of high-quality septa, caps, and vials is equally critical to prevent sample evaporation and contamination. This also acts to minimize blocked syringe needles. The use of high-quality tubing and fittings minimizes solvent or gas leaks, which helps to maintain analytical integrity.

A report published in 2023, entitled “Looking Beyond Routine Lab Equipment Maintenance,” discussed the importance of developing good equipment maintenance schedules as well as developing good working relationships with partners to achieve this (1). The article quoted a 2017 survey from Frost and Sullivan commissioned by Agilent Technologies, and listed instrument maintenance/downtime as a top challenge for 73% of lab managers (2). Regarding unplanned downtime, >75% of the cohort surveyed highlighted this, with sample preparation a key factor in unplanned downtime. Furthermore, they also emphasized that increased utilization of automation and improved after-sales support would help reduce instrument downtime.

Liquid chromatography interfaced with mass spectrometry (LC–MS) is becoming increasingly used in a wide variety of analytical laboratories. Over the last few decades, MS instruments have improved dramatically in terms of analytical sensitivity and specificity. However, analytical results are only as good as what is introduced into the MS interface. To maintain LC–MS performance and prevent blockages and column contamination, samples must be free of particulates. Furthermore, these must have undergone appropriate sample preparation such as filtration, protein precipitation, solid-phase extraction (SPE), or liquid–liquid injection.

The MS interface (electrospray or atmospheric chemical ionization [APCI]) requires desolvation of the LC eluent prior to analyte ionization. To prevent contamination of the source, the LC eluent should not be contaminated with unwanted organics and should not contain non-volatile inorganic buffers such as potassium phosphate. Instead, volatile pH modifiers, such as ammonium acetate, should be employed. Another important component is nitrogen gas, which is used for nebulizing the LC eluent and assisting the desolvation process. The nitrogen must also be free of hydrocarbon interferences, such as phthalates and butylated hydroxytoluene (BHT). As a result, gas traps should be employed to remove such contaminants.

In summary, it can be seen just in these few examples that system downtime causes frustration and wastes money, not only in terms of failing to meet deadlines but also in not being able to maximize the potential of instrumentation. This illustrates the importance of properly maintaining equipment and fostering strong relationships with suppliers to support laboratory efficiency.

For further information, please contact Trajan LPP at 877-725-1007 or email us at lppcustserv@trajanscimed.com. 

References

(1) Welsh, J. Looking Beyond Routine Lab Equipment Maintenance. Lab Manager 2023,https://www.labmanager.com/looking-beyond-routine-lab-equipment-maintenance-31226 (accessed 2025-05-16).

(2) Understanding Key Challenges and Pain Points in the Global Laboratory Market. Agilent Technologies, 2017.https://www.agilent.com/content/dam/about/newsroom/infograhics/pdf/fact-sheet-lab-manager.pdf

James Rudge © Image courtesy of author

James Rudge has a long history in the field of analytical science. He served as an applications specialist in the fields of HPLC, GC, and SPE, a technical director of Neoteryx for four years, and is presently the technical director of automated workflows for Trajan. Rudge has co-authored >20 papers on microsampling and authored a book chapter on VAMS, published in 2024. Furthermore, he has delivered presentations at numerous national and international conferences, and over the years has given many two-day customer separation science training seminars.