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R&D Analysis and Deformulations

New, complex structured, and high-tech macromolecules require precise, reliable and accurate characterization. Realizing the growing demand for advanced macromolecular characterization and the lack of macromelcular expertise in typical service labs, PSS offers state-of-the-art analytical support. Challenges of macromolecular analysis are faced daily at our laboratory. Since our experienced staff devotes time and effort in communicating with customers to identify their specific needs, a high success rate in reaching project objectives is achieved.

Deformulation Analysis
Also known as reverse engineering, deformulation is the separation, identification and quantification of ingredients in a formulation. Deformulation analysis uses a combination of analytical methods and conventional extraction methods to identify and quantify the components of a complex mixture.

This service involves an initial consultation with our analytical services staff to determine the most effective analytical methods to use. A project plan with several milestones will be provided. Methods applied may be all characterization methods PSS provides, including hyphenated techniques as e.g. 2D (2-dimensional) chromatography.

Please note that product deformulation of commercial products is provided for informational purposes only. PSS recommends review of patents, state and federal laws before this information is used.

Example Applications

Additives

Additive Analysis

The quantitative analysis of low molecular weight molecules (such as antioxidants, light stabilizers, plasticizers, lubricants and others) can be performed using liquid chromatography techniques on an analytical scale separated by advanced detection.

Many well known additives are in stock for PSS sample testing to be used as reference material for customer analysis. The additive analysis data is collected in a database containing the following parameters:

  • an FTIR spectrum
  • the GPC/SEC-related retention volume
  • the HPLC retention times with a total of 4 detectors.

The additive analysis includes

  • LC separation, optionally with online FTIR or ESI-MS analysis
  • optional material verification like elemental analysis, ToF-SIMS analysis or others.
  • Extraction of additives according to ASTM D 7210

Aggregation

Protein Aggregation

Aggregation is a major concern during biotherapeutic drug manufacturing, purification, storage and handling as it can change the efficacy of the product.

The combination of GPC/SEC/GFC with light scattering detection is a powerful techniques to study the purity and interactions of proteins and protein-ligand complexes. While GPC/SEC allows the separation and quantification of the associates such as dimer, trimer and more, a MALLS detector can measure absolute molar masses of the various structures.

PSS utilizes aqueous GPC/SEC combined with

  • static light scattering
  • and optional dynamic light scattering

in multi dector setups to detect even low concentrations of oligomers and to determine important protein properties, such as molar masses or radii.

Additional detectors like

  • viscometers, e.g. to distinguish between denaturation and aggregation or
  • fluorescence detectors, e.g. to detect with an improved sensitivity or selectivity

are added depending on the requirements of the application.

The analysis fee for the first sample includes calibration, validation and verification of the system according to the PSS quality system. dn/dc determination is recommended.

Branching

Branching Analysis

Branching of polymer chains strongly affects the physical polymer properties. Long chain branches increases polymer strength, toughness, and the glass transition temperature.

PSS determines long-chain branching using GPC/SEC combined with viscometry and/or multi angle light scattering in a variety of solvents up to 155 °C.

Polyethylene (PE) short chain branching is investigated using HT-GPC with IR detection.

13C NMR is used to determine the nature of an unknown polyethylene (HDPE, LDPE, LLDPE) and can identify and quantify the types of branching present.

Other PSS techniques:

  • CRYSTAF Analysis
  • TREF Analysis

Chemical Composition

Chemical Composition Analysis

In contrast to GPC/SEC Interaction Polymer Chromatography (IPC) allows for separations based on chemical composition or end groups.

PSS utilizes

  • Isocratic/Gradient Chromatography
  • Chromatography under Critical Conditions
  • Chromatography under Limiting Conditions
  • SEC-Grandient
  • Temperature Gradient Interaction Chromatography (TGIC)
  • Temperature Rising Elution Fractionation (TREF)

also as separations in a 2-dimensional setup.

This service involves an initial consultation with our analytical services staff to determine the most effective analytical methods to use.

 

Molar Mass

Molar Mass Distributions

PSS provides GPC/SEC/HT-GPC in in THF, Toluene, DMF, DMAc, NMP, TCM, HFIP, TFE, Water, DMSO, DCB and TCB at temperatures up to 155°C to compare samples and to obtain molar mass averages and molar mass distributions.

In accordance with the requirements of each individual application, we employ various instrument setups, configurations and detectors offering 

  • Conventional GPC/SEC
  • GPC/SEC-Light Scattering (MALLS/RALLS)
  • GPC/SEC-Viscometry
  • GPC/SEC-Light Scattering/Viscometry (Triple/Triple plus detection)
  • GPC/SEC-ESI-MS (only specific solvents)

The analysis fee for the first sample includes calibration, validation and verification of the system according to the PSS quality system. Calibration with customer’s choice of calibration standards is available.

Molar Mass Averages

PSS offers methods to determine molar mass averages only. Batch static multi angle laser light scattering (MALLS/MALS) is the method of choice for determining the molar mass weight average, Mw.
Precise data evaluation requires the knowledge of the sample refractive index increment, dn/dc. PSS provides light scattering Mw determination in a variety of solvents, with or without dn/dc determination using dedicated dn/dc instrumentation at temperatures up to 80 °C.

Other methods for molar mass average determination offered by PSS are MALDI-ToF and 1H-NMR.

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