Best of the Week: The Industry–Academia Collaboration, Sample Injection Troubleshooting

This past week, LCGC International published a variety of articles on hot topics in separation science. Dwight Stoll discusses common problems associated with flow-through needle autosamplers used in modern liquid chromatography, Bob Pirok dives into how statistical validation tools can guide the selection of appropriate calibration models in size-exclusion chromatography (SEC), and Emanuela Gionfriddo discusses the importance of continued collaboration between industry and academia.

This is the Best of the Week.

Leaks and Obstructions: Troubleshooting Common Problems Close to the Point of Sample Injection

In this “LC Troubleshooting” column, Dwight Stoll of St. Adolphus College examines common problems associated with flow-through needle autosamplers used in modern liquid chromatography (LC), focusing on leaks and pressure issues caused by wear of the injection valve rotor.¹ He delves into how the sampler operates, why the polymeric rotor is a mechanical weak point, and how erosion or scratches can lead to internal or external leaks and downstream obstructions.¹ Practical diagnostic clues, such as unexpected solvent puddles or pressure increases, are discussed alongside corrective actions. The article emphasizes rotor replacement, inspection of stator surfaces, and preventative maintenance schedules as the most effective strategies for maintaining autosampler reliability and minimizing instrument downtime.

Is My Calibration Model Reliable? Part I: Validating Calibration Curves in Size-Exclusion Chromatography

In this article, Bob Pirok, an assistant professor of analytical chemistry at the Van ‘t Hoff Institute for Molecular Science (HIMS) at the University of Amsterdam, explains how statistical validation tools can guide the selection of appropriate calibration models in size-exclusion chromatography (SEC).² Using a common polymer analysis question, whether to apply a third- or fifth-order polynomial, he demonstrates the limitations of relying solely on R² and introduce adjusted R² and the F-test to balance model fit against complexity. Through an SEC calibration example, the F-test shows that a fifth-order polynomial provides a statistically significant improvement over a third-order model, while higher orders do not.² The article emphasizes that proper model validation is essential to avoid overfitting and ensure reliable, predictive chromatographic calibrations.

LCGC Blog: How Industry–Academia Collaboration Shapes the Future of Separation Science

In this LCGC Blog, Emanuela Gionfriddo of the University at Buffalo discusses the importance of sustained collaboration between academia and industry, highlighting how it is essential to advancing separation science, driving innovation, and preparing a market-ready workforce.³ Drawing on personal experience and industry perspectives, Gionfriddo shows how partnerships align fundamental research with real-world needs, exemplified by the successful development and adoption of solid-phase microextraction (SPME). Such collaborations improve research relevance, accelerate technology translation, and expose students to practical constraints like robustness, timelines, and regulatory demands.³ She also emphasizes the need for institutional flexibility, adequate funding, and recognition of collaborative efforts to ensure these partnerships remain a defining force in the future of separation science.³

Overcoming Stability Challenges Associated with Determination of Residual Phosphine Ligands in Active Pharmaceutical Ingredients and Their Intermediates Using Liquid Chromatography with Derivatization

This article describes a robust LC method for accurately quantifying residual phosphine ligands from Suzuki–Miyaura coupling reactions in pharmaceutical products. Because phosphine ligands can exist in both non-oxidized and oxidized forms with different ultraviolet (UV) responses and solubilities, direct quantification is unreliable.⁴ This challenge is addressed by derivatizing all residual phosphines to their stable oxidized form prior to analysis.⁴ Using controlled oxidation and a phenyl ultrahigh-pressure liquid chromatography (UHPLC) method with UV detection, the approach eliminates variability, improves accuracy and precision, enabling the reliable control of potentially toxic phosphine impurities in active pharmaceutical ingredients.

Deep In The Heart of Texas: Pittcon 2026

This year, Pittcon is heading to Texas, with the venue being the Henry B. González Convention Center in San Antonio, Texas. Although an unconventional choice, San Antonio’s bioscience, environmental analytics, and defense research footprint aligns with heavy use of chromatography–mass spectrometry (MS) workflows across universities, hospital systems, and industrial testing laboratories in the region.⁵ In this article, we highlight several key aspects to the technical program that conference attendees should look forward to, including sessions on separation mechanisms, stationary-phase selection, sample preparation, robustness, and LC/GC/IC integration with MS for regulated and high-complexity matrices, as well as environmental sessions that will focus on per- polyfluoralkyl substances (PFAS), pharmaceuticals/personal care products, microplastics, and drinking-water toxicity drivers using state-of-the-art analytical and MS techniques.⁵

References

1. Stoll, D. R. Leaks and Obstructions: Troubleshooting Common Problems Close to the Point of Sample Injection. LCGC Int. 2026, 3 (1), 8–11. Available at: https://www.chromatographyonline.com/view/leaks-and-obstructions-troubleshooting-common-problems-close-to-the-point-of-sample-injection
2. Pirok, B. W. J. Is My Calibration Model Reliable? Part I: Validating Calibration Curves in Size-Exclusion Chromatography. LCGC Int. 2026, 3 (1), 12–14. Available at: https://www.chromatographyonline.com/view/is-my-calibration-model-reliable-part-i-validating-calibration-curves-in-size-exclusion-chromatography
3. Gionfriddo, E. LCGC Blog: How Industry–Academia Collaboration Shapes the Future of Separation Science. LCGC International. Available at: https://www.chromatographyonline.com/view/how-industry-academia-collaboration-shapes-the-future-of-separation-science (accessed 2026-02-06).
4. Sweatman, J. Overcoming Stability Challenges Associated with Determination of Residual Phosphine Ligands in Active Pharmaceutical Ingredients and Their Intermediates Using Liquid Chromatography with Derivatization. LCGC International. Available at: https://www.chromatographyonline.com/view/overcoming-stability-challenges-associated-with-determination-of-residual-phosphine-ligands-in-active-pharmaceutical-ingredients-and-their-intermediates-using-liquid-chromatography-with-derivatization (accessed 2026-02-06).
5. Matheson, A. Deep In The Heart of Texas: Pittcon 2026. LCGC International. Available at: https://www.chromatographyonline.com/view/is-my-calibration-model-reliable-part-i-validating-calibration-curves-in-size-exclusion-chromatography (accessed 2026-02-06).