News from LabRulezLCMS Library - Week 27, 2026

Our Library never stops expanding. What are the most recent contributions to LabRulezLCMS Library in the week of 29th June 2026? Check out new documents from the field of liquid phase, especially HPLC and LC/MS techniques!

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This week we bring you application notes by Agilent Technologies and Metrohm and posters by Shimadzu/ASMS, Thermo Fisher Scientific/ASMS and Waters Corporation/ASMS!

1. Agilent Technologies: Integrated Structural and Functional Characterization of a GLP-1 Analogue Using LC/MS and SPR

• Application note
• Full PDF for download

GLP-1 RAs have emerged as one of the most impactful classes of peptide therapeutics in modern medicine. Initially developed for glucose control in type 2 diabetes, GLP1 RAs are now widely recognized for their substantial benefits in weight management, cardiometabolic health, and organ‑protective effects.1 Their rapid adoption has accelerated innovative efforts, driving the development of next-generation analogs with extended half-lives, enhanced potency, and improved stability. As manufacturers explore new sequence variants, chemical modifications, and formulation strategies, the need for early and comprehensive characterization becomes essential. These peptides often incorporate lipidation, PEGylation, amino acid substitutions, or other structural changes intended to modulate pharmacokinetics and receptor engagement.2 However, such modifications can also influence peptide folding, degradation pathways, aggregation, or target binding in ways that are not always intuitive. Understanding how structural integrity translates into functional activity is therefore critical for guiding design decisions, optimizing stability, and ensuring product comparability throughout development. 

This application note presents an integrated analytical workflow combining an Agilent 1290 Infinity II bio LC system, an Agilent 6545XT AdvanceBio LC/Q-TOF, and a Nicoya Digital Surface Plasmon Resonance (digital SPR) system to provide a holistic assessment of GLP-1 RA structure and function. LC/MS enables detailed structural profiling—including mass confirmation, impurity analysis, and degradation monitoring— while digital SPR delivers real-time, label-free measurements of GLP-1 receptor binding kinetics. When used together, these orthogonal techniques allow developers to directly correlate chemical modifications or degradation products with changes in biological activity. In several cases, this combined approach reveals unexpected disconnects between structural homogeneity and receptor binding behavior, underscoring the value of functional assays alongside structural characterization. By integrating LC/MS and digital SPR, biopharmaceutical scientists can streamline early-stage screening, support stability and forced degradation studies, improve comparability assessments, and gain deeper insight into structure-activity relationships. This workflow aligns with current industry trends toward faster development timelines and more robust characterization strategies, enabling confident decision-making from early discoveries through development and quality control.

Experimental

Analytical equipment 

• An Agilent 1290 Infinity II bio LC system included the following modules:
• Agilent 1290 Infinity II Bio high-speed pump (G7120A) 
• Agilent 1290 Infinity II Bio multisampler (G7137A) 
• Agilent 1290 Infinity II multicolumn thermostat (G7116B) 
• Agilent 6545XT AdvanceBio LC/Q-TOF (G6549AA) 
• Digital SPR 16-Channel Instrument with Nicosystem Pro Software (DSPR16-PRO) 
• 16-Channel Carboxyl Cartridge (KC-CBX-CMD-16) 

Software and data processing 

• Agilent MassHunter data acquisition software, version 11.0 
• Agilent MassHunter BioConfirm software, version 12.1 
• Agilent MassHunter Qualitative Analysis, version 12.0 
• Digital SPR Nicosystem User Portal

Conclusion 

The integrated workflow described in this study—combining LC/MS for structural analysis with SPR for ligand binding assessment—provides an important framework for understanding structure-function relationships in GLP-1 analogues and their receptor. 

The results generated using this integrated approach contribute valuable insights to the existing knowledge base for these molecules. The study exposed that cleaving of the peptide caused it to completely lose its function, highlighting the risk of degraded species in the final product. Meanwhile, we showed that oxidation, a common degradation pathway for peptides, had no impact on the function of liraglutide, perhaps reducing risk in some manufacture and storage approaches. 

Beyond supporting fundamental characterization, this workflow offers meaningful advantages to the biopharmaceutical industry, helping optimize candidate selection and refinement during both discovery and development.

As GLP-1 RAs continue to expand in therapeutic scope and market impact, advanced analytical solutions will be essential for ensuring patient safety and accelerating access to innovative therapies.

2. Metrohm: Potentiometric analysis of rare earth elements (REEs)

Accurate and precise back-titration of rare earth elements with the copper-selective electrode

• Application note
• Full PDF for download

Rare earth metals are comprised of 17 elements including the lanthanide series as well as the elements scandium and yttrium. These REEs are primarily used in batteries, nanotechnology, photovoltaics, medical technology, aerospace, and military technology. The concentrations of REEs in ore and rock must be measured to determine the viability of a rare earth deposit. After crushing, the ores are dissolved, separated, and purified, and the REEs, along with other elements, are monitored throughout this stage. Determining the mass fraction of rare earth metals here is crucial and involves significant effort.

This Application Note presents a rapid and precise back-titration method using the Cu-ISE, which clearly separates a number of rare earth metals, even when they are combined with other elements, and enables them to be analyzed with nearly 100% recovery.

EXPERIMENTAL 

The determination is carried out using an OMNIS Sample Robot S – WSM, an OMNIS Professional Titrator equipped with OMNIS Dosing Modules, as well as a copper-selective electrode (Figure 1). An appropriate amount of sample is weighed into the titration beaker, and acetate buffer as well as standardized EDTA solution are added. After a waiting time, the solution is titrated until after the first or second equivalence point with standardized CuSO4 solution.

CONCLUSION 

Back-titration is a cost-effective and precise alternative to conventional analytical methods, such as ICP, for determining the presence of rare earth elements. As a method of determination, potentiometric titration is flexible in handling the wide variety of REE minerals. Thanks to optimization of the analytical matrix and the use of complex chemistry, it can even separate certain REEs from each other in mixtures. The automated system with the OMNIS Sample Robot S – WSM equipped with an OMNIS Titrator, OMNIS Dosing Modules, and copper-selective electrode, impresses with its high level of professionalism and offers flexible analyses combined with high-end software.

3. Shimadzu / ASMS: LC-MS/MS QTOF analysis of river water identifies contaminants of environmental concern by non-targeted profiling

• Poster
• Full PDF for download

Identifying contaminants of environmental concern in water-based epidemiological investigations has provided mechanistic insight into wastewater treatment performance and transformation processes. Both targeted and non-targeted approaches have been employed to detect emerging contaminants potentially originating from treated or untreated wastewater discharges, particularly under storm-driven overflow conditions events. In this study, river water grab samples were collected across tidal and freshwater environments systems. High-resolution LC/QTOF with DIA-MS/MS was applied using a direct injection reversed-phase workflow method. Data analysis leveraged novel non-targeted profiling software to identify differences in the distribution of detected components between and within defined sample groups.

Materials and Methods

Reversed phase LC Separation: 

Nexera X2 

• Column: Shim-pack Velox Biphenyl (100 x 2.1 mm, 2.7 µm); 
• column temp. 40 ºC, 
• flow rate: 0.3 mL/min, 17 min total analysis time. 
• Binary gradient; methanol:water gradient with 2 mM ammonium formate and 0.002% formic acid 

High resolution QTOF analysis: 

• LCMS-9050 
• MS scan m/z 100-1000, 100 msec scan time. 
• MS/MS DIA 35 consecutive scans (m/z 100-500 20 Da precursor isolation width, m/z 500-1025 35 Da precursor isolation width), 25 msec scan time (0.925 sec total cycle time)

Conclusions 

Insight Profiler non-targeted analysis software was applied to the analysis of urban river water using a direct injection method. 

The results highlight the complex and dynamic changes occurring in urban river water in which a single source can have far reaching influences downstream however global trends can still identify contaminants such as HMMM with high confidence.

4. Thermo Fisher Scientific / ASMS: Low-resolution FAIMS for increased peptide coverage in low-load and single-cell proteomics

• Poster
• Full PDF for download

Field Asymmetric Ion Mobility Spectrometry (FAIMS) is widely used in low-input and singlecell proteomics to improve selectivity and reduce chemical background. However, FAIMS operates as a front-end ion filter, and using a single compensation voltage (CV) can reduce peptide coverage due to ion filtering. Increasing the number of CVs improves coverage but lengthens duty cycle and compromises quantitative precision, which is especially problematic for limited samples. FAIMS resolution is influenced by electrode temperature, affecting ion mobility and CV peak width. Here, we investigate whether deliberately lowering FAIMS resolution by electrode temperature modulation can increase ion transmission and improve identification rates and quantitative robustness in discovery proteomics, while retaining the practical advantages of single-CV operation.

Materials and methods

LC-MS configuration 

Samples were analyzed using the Thermo Scientific Vanquish Neo UHPLC system. Peptides were loaded on a trapping column (Thermo Scientific PepMap C18, 5 mm × 300 μm i.d.) using 0.1% TFA for the loading buffer. Peptides were separated on an Aurora RapidTM 8×75 XT C18 nanoflow UHPLC column at 50 °C. For MS measuring, the Thermo Scientific Orbitrap Astral mass spectrometer equipped with a Thermo Scientific FAIMS Pro Duo interface and a Thermo Scientific EASY-Spray source was coupled to the LC. A compensation voltage of –48 V and a carrier gas flow of 3.5 L/min was chosen based on previous results. 

MS1 spectra were recorded using the Orbitrap analyzer at a resolution of 240,000 from m/z 400 to 800 using an automatic gain control (AGC) target of 500% and a maximum injection time of 100 ms. MS2 scans were acquired in the Astral analyzer, the precursor range was set to 400 - 800 m/z and the AGC target to 500%. Single cells were measured with DIA window size of 20 Th and maxIT 40 ms. The Hela dilution series were acquired with optimized method parameters based on the peptide load on column. The DIA isolation widths and maxIT were adjusted as specified in the respective graphs.

Conclusions 

This study demonstrates that low-resolution FAIMS significantly increases peptide and protein identifications from low-load samples. By broadening the compensation voltage window, it enhances ion transmission, improving identifications in low-load HeLa digests and single cells. In line, higher charged and higher m/z ions showed an improved identification rate compared to standard resolution FAIMS. The resulting sensitivity boosts detection of low-abundance proteins and strengthens quantification quality, which is crucial for single-cell proteomics. Low-resolution FAIMS also raises ion counts in MS1 and MS2, improving quantitative precision - we consistently observed lowered CoVs of samples measured with a lower outer electrode temperature. 

These findings provide a simple, practical tweak: adjusting FAIMS resolution delivers better results without additional hardware or changes to data processing, making it a costeffective, straightforward enhancement.

5. Waters Corporation / ASMS: Natural Food Supplements: Characterization using LC/MS – Ashwagandha, Turmeric and Ginger Examples

• Poster
• Full PDF for download