News from LabRulezICPMS Library - Week 48, 2025
LabRulez: News from LabRulezICPMS Library - Week 48, 2025
Our Library never stops expanding. What are the most recent contributions to LabRulezICPMS Library in the week of 24th 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: Precursor Detection Using an Agilent Resolve Tactical Handheld Raman Analyzer
- Application note
- Full PDF for download
Chemicals used in the illicit manufacturing of narcotic drugs and psychoactive substances are known as "drug precursors". Drug precursors include chemicals that are one reaction away from being the drug (e.g. 4-ANPP to fentanyl), chemicals that are used in a wide range of legal applications from fragrances (e.g. benzaldehyde) to solvents (e.g. toluene), and chemicals that are multiple reaction steps away from the drug itself, sometimes called a "pre-precursor". The resulting "pre-precursor" may be sufficiently different from the main precursor that it circumnavigates legislation, mobilizing drug synthesis to any country.
The Agilent Resolve tactical handheld Raman analyzer uses spatially offset Raman spectroscopy (SORS) technology to identify hazardous materials, explosives, and narcotics concealed behind single and multiple barriers. These barriers can include colored and opaque plastics, glass, paper, card, wrapping, and fabrics. The combination of SORS, high data quality, reduced fluorescence interference, and a library continuously updated with new psychoactive substances makes the Resolve a powerful tool in the detection and identification of controlled substances. As of library version 43, over 80 different precursors can be identified using Resolve.
Conclusion
The Agilent Resolve tactical handheld Raman analyzer can be used for the fast, direct identification of drug precursors in the original packaging. Direct analysis using the Resolve minimizes the risk of accidental exposure to the compounds by law enforcers.
2. LECO: Determination of Nitrogen in Plastics
- Application note
- Full PDF for download
The plastics industry is currently one of the largest manufacturing industries worldwide and shows continued growth. Plastics have a wide array of applications such as packaging, medical supplies, automotive parts, insulation, and many more. Plastics consist of a wide range of synthetic or semi-synthetic materials, such as polyethylene terephthalate (PET), which are composed of polymers. Compounds containing Nitrogen are commonly used in the manufacturing of plastic materials such as initializers, plasticizers, stabilizers, and various polymerization modifiers. These compounds play an important role in the physical and mechanical properties of the plastic material. The determination of Nitrogen is crucial in the material characterization and quality control procedures for the manufacturing and molding process of plastic materials.
The classical method utilized for Nitrogen determination in organic materials is the Kjeldahl method which involves sample digestion, distillation, and ammonia determination typically by titration. This method involves time-consuming sample preparation and the use of hazardous materials. The LECO FP928 is a Nitrogen determinator that utilizes an automated Dumas combustion method and provides accurate and precise results in approximately five minutes. This eliminates involved sample preparation and the use of hazardous materials resulting in a cost-effective method for the quality control of plastic production.
Instrument Model and Configuration
The LECO FP928 is a macro combustion Nitrogen determinator that utilizes a pure Oxygen environment in a high-temperature horizontal ceramic combustion furnace, using ceramic or Nickel combustion boats designed to handle macro sample masses (~1.0 g). A thermoelectric cooler removes moisture from the combustion gases before they are collected in a ballast. The gases equilibrate and mix in the ballast before a representative aliquot (3 cm3 or 10 cm3 volume) of the gas is extracted and introduced into a flowing stream of inert carrier gas (Helium or Argon) for analysis. The aliquot of gas is carried through a heated reduction tube, filled with Copper, to convert Nitrogen Oxide combustion gas species (NOx) to Nitrogen (N2). The aliquot gas is then carried to a thermal conductivity cell (TC) for the detection of Nitrogen (N2)
TYPICAL RESULTS
Data was generated utilizing a linear, force through origin calibration using 502-602 Ammonium Solution (0.1% N). The calibration was verified using 502-601 Ammonium Solution (0.01% N). All reference materials and samples were weighed and analyzed at ~1.0 g. Approximately 2 ml of deionized water was added to the samples prior to analysis to reduce sooting.
3. Shimadzu: Quantitative Analysis of Antacid (Aluminum) in Drug by EDX (EDX-7200)
- Application note
- Full PDF for download
User Benefits
- The titration method and atomic absorption spectrophotometry require complex sample preparation, but with EDX, analysis is possible with simple sample preparation.
- The analysis time is only a few minutes, contributing to work efficiency.
- Repeatability is good, and highly accurate results can be obtained.
Aluminum (Al) compounds such as aluminum hydroxide gel and synthetic hydrotalcite are widely used as antacids because they have the effect of neutralizing excess stomach acid and reducing irritation of the stomach wall. At pharmaceutical manufacturing sites, the titration method or atomic absorption spectrophotometry is generally adopted for control of antacids in drug products, but these analytical methods have the problems shown in the following Table 1.
Because the energy dispersive X-ray fluorescence spectrometer (EDX) enables analysis with only simple sample preparation, and the analysis time is also short, at a few minutes per sample, higher analysis efficiency can be expected. For this reason, EDX has attracted attention as an alternative analytical method to the titration method and atomic absorption spectrophotometry. This article introduces an example of an analysis of an antacid (Al) used in commercially-available drugs.
Comparison of Unknown Sample Analysis by EDX with Titration Method
Three unknown samples were prepared (n = 3 for each sample material), and a quantitative analysis was conducted. Table 4 shows the results. The relative error of the average values obtained by the EDX method to the quantitative values obtained by the titration method showed a satisfactory correlation of 3.5 % or less.
A significance test of the difference in the quantitative values by the two methods was carried out assuming a significance level of 5 %. Because the null hypothesis “no difference” is not rejected, it cannot be concluded that there is a difference between the two methods.
EDX is a potential alternative to the titration method, and the evaluation of that possibility is based on a total judgment, including the number of unknown sample materials, the control range of the amount of addition, the variance between the two methods(homogeneity of variance test) and other factors
Conclusion
- EDX has the following advantages:
- Analysis is possible with simple sample preparation.
- Short analysis with a few minutes.
- High repeatability.
- Easy analysis operation.
EDX is expected to be used as an alternative to the titration method in research and development and quality control work.
4. Waters Corporation: Subvisible Particles: Why Don’t I Just Filter My Biologic Samples?
- Application note
- Full PDF for download
Filtration of a therapeutic is often cited as a key method to remove particles generated during the manufacturing process. From ultrafiltration and diafiltration (UF/DF) to tangential flow filtration (TFF), several methods are employed throughout the bioprocess to remove aggregates and other product impurities.1 While filtration removes preformed particles, including subvisible particles (SVPs), it does not account for the inherent instability of biologic samples, and thus subvisible aggregates can be generated over time even after filtration2 . In addition, the expansion in the complexity of biologic therapies leads to additional challenges during the manufacturing process from purification to filtration. In some cases, filtration cannot be applied as is the case with cell-based therapies. Therefore, all biologics need to be formulated to be stable over the long term, regardless of filtration.
In this application note, we use Aura® System and backgrounded membrane imaging (BMI) to explore the effect of filtration on three different biologic formulations, two therapeutic proteins and a lipid nanoparticle (LNP) formulation. We analyze for the presence of SVPs in these three sample types immediately after filtration and sequentially over a two-week period. Here, we learned that filtration greatly reduces the original SVP content, but SVP formation continues to increase as a function of time with a rate that is sample dependent.
Results and Discussion
Impact of Filtration on SVP Counts
In this small study across the three different samples tested (Protein 1, Protein 2 and LNPs), a significant amount (>90%) of subvisible particles (>0.2 µm) were removed by a single round of filtration using a 0.2 µm syringe filter. Interestingly, filtration did not remove all particles larger than the size threshold of the filter, and thus highlights the limited efficiency on SVP clearance (Figure 1a). An explanation for this includes that a single round of filtration itself is imperfect and often biologics are filtered more than once and through various methods.
Conclusion
Sample filtration is used as an integral part of the bioprocess to remove extraneous particles from the final drug product; however, it does not fix the inherent stability of biomolecules. Stability itself is governed by thermodynamics: time, temperature and the chemical nature of the sample and its formulation. Subvisible particles are the most important stability parameter: they highlight the presence of large physiologically relevant aggregates with the capacity to affect both safety and efficacy of any final drug product. What we have shown is that cleaning the final product using filtration doesn’t result in a stable particle-free sample risking drug efficacy and patient safety. Applying Aura System in your workflow enables rapid long-term stability assessment via a low volume, high throughput assay.
