News from LabRulezICPMS Library - Week 47, 2025

Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 17th November 2025? Check out new documents from the field of spectroscopy/spectrometry and related techniques!

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This week we bring you application notes by Agilent Technologies, LECO, Shimadzu and Waters Corporation!

1. Agilent Technologies: Microplastics Characterization in Carbonated Beverages and Apple Juice by Laser Direct Infrared

• Application note
• Full PDF for download

The widespread use of plastic materials in the production, packaging, and distribution of foods and beverages has raised growing concerns about microplastic contamination. Popular beverages bottled in plastic-containing packaging are increasingly recognized as potential contributors to dietary microplastic exposure. Studies have reported microplastic particles in commercial mineral water and soft drinks, often introduced through bottling operations, cap abrasion, or migration from plastic containers and multilayer packaging materials.^1-4

Carbonated beverages and apple juice are commonly packaged in a variety of container types, including polyethylene terephthalate (PET), polyethylene (PE), aluminum cans, glass bottles, and multilayer cartons. Microplastics may shed into the product from the packaging materials or be generated during the preparation and filling stages. Factors like high-speed bottling, carbonation pressure, and storage conditions can further accelerate the release of microplastics into the liquid matrix.^2,5 

Detecting microplastics in complex beverage formulations presents significant analytical challenges, primarily due to the presence of organic matter and mineral constituents in these products. Traditional techniques such as micro-Fourier Transform Infrared spectroscopy (µFTIR) and µRaman spectroscopy can effectively identify and characterize microplastics in beverages, typically following digestion and density separation to avoid matrix-related interferences. Also, method development and sample run times for both techniques are often labor-intensive and low-throughput, limiting the number of samples that can be processed within a given timeframe.

To address these limitations, the highly automated Agilent 8700 Laser Direct Infrared (LDIR) chemical imaging system (Figure 1) significantly improves sample throughput, enabling the rapid, accurate detection of microplastics in complex matrices following direct filtration. The system uses a Quantum Cascade Laser (QCL) that allows rapid and precise scanning across the mid-infrared (MIR) fingerprint region (1,800 to 975 cm–1), providing high-quality spectral data. It also provides high-quality imaging data using two high‑quality visual cameras that are fully controlled by the Agilent Clarity software. The software also includes preset methods such as Particle Analysis to simplify the analysis, as well as data reporting tools to aid interpretation and decision-making.

This application note demonstrates the use of the 8700 LDIR for the characterization of microplastics extracted from commercially available carbonated beverages and apple juice packaged in various container types. The particles were analyzed directly on aluminum-coated filters.

Results and discussion

Carbonated beverages 

To locate particles and define their boundaries, the 8700 LDIR automated Particle Analysis workflow conducted an initial rapid scan over a selected area (~16 mm diameter per filter) using a fixed wavenumber (1,442 cm–1). Following detection, the system automatically acquired full infrared spectra for each particle across the spectral range. These spectra were then matched in real time against the Microplastics Starter 2.1 spectral library for identification. 

Although a residue layer was observed on the aluminum‑coated filters following filtration of the carbonated beverages, it did not interfere with the LDIR's particle detection or identification capabilities (Figure 3). As shown in Table 2, microplastics were identified in all three beverage samples, with particle counts of 50, 39, and 384 for samples 1, 2, and 3, respectively (HQI > 0.85). 

PVC was detected across all container types, such as rPET (37 particles), aluminum can (25 particles), and glass, which unexpectedly exhibited the highest particle count (227 particles). This may be attributed to the cap liner material (often a multilayer seal designed to prevent oxygen or moisture ingress) or potential cross-contamination during bottling through piping systems. PET microplastics were also identified in all samples, with particle sizes ranging from 20 to 500 µm (Table 2)

Conclusion 

This study highlights the advantages of using the Agilent 8700 LDIR chemical imaging system for characterizing microplastics in carbonated beverages and apple juice contained in various types of packaging. When consumed, these drinks may serve as potential sources of microplastic exposure. 

The 8700 LDIR enabled a direct on-filter analysis approach that significantly simplified the workflow by eliminating traditional preparation steps such as digestion and density separation, speeding up the analysis. The on-filter method reduced the potential for sample contamination while enhancing recovery rates and sample representativeness by enabling filtration of the entire product volume. 

The two-position filter holder facilitated the automated, sequential analysis of both a procedural blank and sample under identical conditions, supporting an accurate quality control process. 

The automated Particle Analysis method in the Agilent Clarity software was used to detect and process data from microplastics contained on the two filters. The software automatically searched the microplastics IR spectral library to identify the polymer type of each particle, providing a "Hit Quality Index" confidence rating for each result. Using this fast and automated workflow, the 8700 LDIR characterized the microplastic content of the beverages with minimal operator input. 

The detailed chemical and physical information generated for each particle by the 8700 provides valuable insight into microplastic pollution, particularly in food and beverages. This data supports the identification of potential contamination sources and facilitates assessment of their broader environmental and human health impact of microplastics.

2. LECO: Determination of Moisture and Ash in Graphite

• Application note
• Full PDF for download

Graphite is a stable form of carbon that exists in nature or can be synthetically produced. Graphite has many applications in our daily lives including its use in pencils, lubricants, electrodes, batteries, and carbon fiber. Synthetic graphite is a man-made substance manufactured by the high temperature processing of amorphous carbon materials. The types of amorphous carbon used as precursors to graphite are many, and can be derived from petroleum, coal, or natural and synthetic organic materials. Synthetic graphite is more pure in terms of carbon content and tends to behave more predictably. Graphite is a very popular material used in electronics and batteries due to its great conductive properties. It is the most commonly used substance to serve as the anode material in lithium-ion batteries due to its relatively low-cost and its energy density. Graphite in the form of carbon fibers is nearly five times stronger than steel and three times lighter. Therefore, carbon fibers and sheets have a wide variety of uses in the manufacturing world, including the automotive, aerospace, military, sporting equipment and construction industries. 

The purity or grade of graphite is directly related to its suitability for different applications. The purer the graphite, the lower the ash content. The ash values of graphite samples can be utilized to compare the relative purity of various grades of graphite. Therefore, ash determination in graphite is a useful quality control process in the graphite industry.

Instrument Model and Configuration 

Thermogravimetric analysis (TGA) is an analytical technique in which changes in sample mass, due to changes in the physical and chemical properties of materials, is measured as a function of temperature and/or time. TGA is commonly used to determine selected characteristics of materials that exhibit either mass loss, or gain, due to decomposition, oxidation, or loss of volatile materials such as moisture. Macro TGA systems typically use a nominal one-gram sample mass to allow more accurate mass change measurements in heterogeneous materials. 

The LECO TGA801 is a macro thermogravimetric analyzer designed to determine moisture, volatile and ash content of materials by measuring the change in mass of the sample as a function of the oven temperature while controlling the atmosphere and ventilation rate. The TGA801 allows up to 19 samples to be analyzed simultaneously.

3. Shimadzu: Determination of Additive and Trace Elements in Lubricating Oil Using ICP-MS

• Application note
• Full PDF for download

User Benefits

• Metal elements in lubricating oil can be accurately analyzed by dilution with organic solvents.
• Solvent-resistant peristaltic pump tubing enables the addition of internal standard elements in-line, even for organic solvent analysis, thereby eliminating the need for manual addition.

Organic metal compounds are added to lubricating oil to provide various functional properties. Therefore, monitoring the concentrations of these additivesisimportant for ensuring quality control. In addition, the analysis of wear metals and contaminant metals in lubricating oils (engine oils) used in automobiles and shipsis a crucial method for assessing the condition of the engine. Traditionally, these analyses have utilized ICP Optical Emission Spectrometry (ICP-OES) as outlined in ASTM D4951-141) and ASTM D5185-182). However, for the analysis of trace metal elements that are difficult to detect with ICP-OES, the more sensitive ICP massspectrometry (ICP-MS) is more suitable. 

In this Application News, lubricating oil was diluted with organic solvents, and the additives and trace elements in the oil were analyzed using the ICP-MS 2050 (Fig. 1). To verify the accuracy of the analytical results,spike recoveries were also evaluated.

Conclusion 

In this Application News, the analysis of metal elements in lubricating oil was performed using the ICPMS-2050 with the organic solvent injection system. Good spike recoveries were achieved, confirming that trace metal elements in lubricating oil can be accurately quantified with a simple sample preparation involving only dilution with organic solvents. Since it is possible to analyze without the complex procedures required for acid decomposition, the risk of volatilization or contamination of the analytes during the sample preparation process is reduced. Additionally, the use of solvent-resistant peristaltic pump tubing enables the in-line addition of internal standard elements, further reducing the time required forsample preparation.

4. Waters Corporation: AAV Aggregate Quantitation and Identification with the Aura System

• Application note
• Full PDF for download

Adeno-associated viruses (AAVs) have transformed gene therapies by enabling the targeted delivery of curative genetic payloads.1 However, the amount of AAV material available is consistently in short supply due to its inherently expensive, time-consuming, and laborious production process.¹ Regardless, critical quality attributes still need to be measured throughout development. Subvisible particles are perhaps the most important parameter to monitor because they lead to adverse immunogenicity events. Thus, this data must be provided to the FDA during the review process.² Additionally, measuring the stability of the capsid is an indicator of the shelf life and efficacy of the product. 

The Aura™ platform is the first ultra-low-volume, subvisible particle analysis system that quantitatively characterizes the stability of different AAV serotypes with as little as 5 µL. This application note demonstrates how several AAV serotypes tend to form large, subvisible aggregates that cannot be predicted using other techniques. It explores the stability and subvisible particle formation in AAV2, AAV5, and AAV8 under different stress conditions and compare the results to stability predictions made by differential scanning calorimetry. In addition, it analyzes the nature of the subvisible aggregates using complete morphological analysis and fluorescence membrane microscopy (FMM) using as low as 10 µL per AAV sample.

Results and Discussion 

Subvisible particle aggregation was observed as a function of serotype and stress conditions with as little as 10 µL per sample (Figure 1). When unstressed AAV samples (samples processed and measured directly from the vial) were compared to each other, the AAV2 (Figure 1a) sample contained less subvisible particles compared to the AAV5 (Figure 1b) and AAV8 (Figure 1c) samples, respectively. Increased levels of protein aggregation were observed in all AAV samples after stressing the samples at 73 °C for 2 hours, though each serotype produced aggregates with different morphologies. The stressed AAV2 produced well-defined small to large granular particles (Figure 1d) while stressed AAV5 contained large fibrillar structures (Figure 1e). The stressed AAV8 sampled (Figure 1f) denatured into a film-like matrix that spread throughout the membrane, resulting in no discernable subvisible particles but showing complete sample degradation.

The Aura System detects and distinguishes the particles formed in different AAV serotypes, both in unstressed and stressed samples. The data generated demonstrated that neat, unstressed samples contain visible aggregates and that each AAV serotype forms different types of aggregates, from granular (AAV2), through fibrillar (AAV5) to fully denatured films (AAV8), when they were thermally stressed. Thermally stressing the AAV2 samples at 73 °C for 2 hours produced a significantly lower number of particles compared to the AAV5 and AAV8 samples, respectively

Conclusion 

The Aura platform delivered both quantitative and qualitative protein aggregation information for several AAV serotypes under different conditions with volumes as low as 10 µL per sample. In comparison, this is <30X the volume typically required with the most advanced low volume flow imager and <1000X lower volume than light obscuration systems. The ability to image brightfield (BMI) and fluorescence (FMM) images at the same time also defines what is protein and what is not in the ThT-stained samples. The Aura System helps characterize your AAV samples with the lowest volume requirements, the highest throughput (<1 minute/sample) and reveals the greatest insights into their stability.