In our previous blog posts from our analytical testing series, we covered the many aspects of why, what and types of analytical tests. In our final post of the series, we cover the HOW. To run analytical testing, you need one or more test methods. These serve as the blueprint for how to run tests. Methods define the equipment, procedure and calculations needed to achieve satisfactory results for the test specimen. Some customers already have these created and send with their samples. For those who haven’t created methods, our team can develop them for you.

What are test methods?

As mentioned, test methods serve as a blueprint for analytical testing but also are used to validate the product production process. They identify what is in a material, how to assemble the material, or how to produce a product. We typically categorize test methods as analytical methods and process methods.

Analytical methods are conducted within the lab environment with specialized equipment and serve several functions:

  • Detect, identify, characterize and quantify chemical compounds within a test specimen or sample
  • Analyze mass, chemical composition, molecular structure, radioactivity, interactions between molecules, etc.
  • Ensure safety and effectiveness, provide quality control and comply with regulatory standards

Process methods, on the other hand, detail the steps and specifications along the chemical manufacturing journey and are designed to:

  • Optimize chemical reaction conditions and the scale-up process
  • Ensure the product’s quality, safety and efficiency
  • Comply with regulatory requirements for product purity, labeling and safety
  • Minimize environmental impact

How are test methods created?

When designing analytical methods, development begins with defining the goal or objective, which contributes to defining the techniques or equipment and experimental conditions. The final step is validation to ensure the method produces the desired results and can be replicated.

Some questions to ask when defining goals include:

  • Do you want to test for the presence of the active ingredient (AI)?
  • Do you need to understand how other components within the product impact the AI’s purity?
  • Do you need to confirm the amount of the AI present?

These goals will help in determining which techniques and equipment to use. Consistency and procedure are critical in analytical testing. Techniques like High-Performance Liquid Chromatography (HPLC), Gas Chromatography (GC), and Mass Spectrometry (MS) provide assurance that each time a test is run, it is repeatable.

Validation helps refine the parameters and techniques to ensure each time the test is run, it is consistent. This phase of the process may take some time. “There is a lot of research and then a lot of trial and error on the HPLC, GC just to make sure the chromatography looks good and the method is working properly,” Victoria Maskule, our analytical chemist, explained.

Process development follows a similar path after the product or formulation has been created. There are a number of factors to consider when creating the process method, including:

  • Equipment from mills to vessels
  • Reaction time, temperature and pressure
  • Quality control measures
  • Energy and waste management

Once defined, the process should be optimized. This usually first happens in the lab and involves running the product through the process to identify where efficiencies can be improved and costs reduced. Process optimization often involves adjusting the reaction conditions, catalysts and process parameters. After success in the lab, the process should be tested in a pilot plant and scale-up environment.

Our pilot plant system features three different volume batch systems ideal for simulating the commercial scale volumes for various product types. The pilot plant testing is designed to create a commercial-ready process so the product can be transitioned to full-scale production without risking quality, safety or efficacy. The final step is validating the process to ensure it can consistently produce the product to meet desired specifications.

Throughout a formulation or product’s lifecycle, the analytical and process methods should be evaluated for improvements or adjustments. New techniques or more advanced equipment may be developed, alternate sources of ingredients may be found, improvements or adjustments may be made to products. These would all require potential refinement to the methods.

Connect with CJB Applied Technologies for your method development needs

The many steps of preparing a product for commercialization can be overwhelming, costly and time-consuming. For companies with a deep R&D pipeline or limited staffing expertise, preparing the necessary test methods for analytical and stability testing, as well as commercial production, can be a challenge. Our team is backed by decades of method development, analytical, stability and formulation experience to help companies fill their capacity gaps. In addition, our pilot plant team supports your scale-up needs through commercialization. We use our pilot plants to ensure your formulation is tested at sufficient volumes to mimic commercial production so there are no issues when you transition to full-scale production. We also use our pilot plants for custom or small-volume batches. And if you are experiencing production capacity constraints, our team can seamlessly transition your product to our sister company CJB Industries for commercial production.

Are you creating synthetic or biological products and need analytical testing support, such as stability testing, clean out validation, retain evaluation and more? Contact us today. You can tap into any of our services independently of the others – product development, analytical testing, method development, scale up and commercialization needs.

Also, be sure to check out previous blog posts in this series: