Analytical Contract Lab Providing Particle Size and Characterization Testing Services

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Evolution of Particle Characterization Instrumentation – Advancing Test Methods for Upgraded Instrumentation

by Rebecca Wolfrom

Over time, advancements in technology have led to changes in many aspects of our lives. These advancements include improvements to tried-and-true scientific instruments, including those in the science of particle characterization.

Academic research continues to hone theories, and in turn the theories are built into software codes, hardware configurations, and even CFR Part 11 compliance programming. This means the instruments used while establishing a test method may be superseded by a newer model. In some fields, this may have a minimal effect on test results. But in particle characterization, it can mean significant differences in sensitivity, detection range, sample handling, or other factors. Any of these could mean a change in result relative to your specification – and no one likes surprises when it comes to meeting a specification.

This is where Particle Technology Labs comes in. At PTL, we’ve used particle characterization instrumentation all day, every day, for over 25 years. This translates to a high level of familiarity with the different techniques, theories, and upgraded equipment models. We stay up-to-date with the latest offerings from the manufacturers and are here to help with applying your method to the ever-evolving instrumentation.

Manufacturers can make a multitude of changes to their hardware in a single model upgrade. Such changes can include extended detection ranges, reconfigured flow paths, increased sensitivity, modified data capture rates, and automated sequences, to name just a few. While these features are often marketed as user-friendly benefits, they can present challenges when a body of work has already been established using a prior model. Some of the most interesting projects at PTL are those where the chemists investigate the effects of the new settings on the results and experiment until the puzzle is solved.

To meet the challenge presented by new instrument models, PTL first conducts internal studies to establish statistical equivalency between the legacy and new instrument model using reference materials. Each resulting report is available upon request to clients who are evaluating the need to make a move. Since the equivalency is demonstrated using model materials only, it is important to evaluate the results specific to the client’s own material. To do so, we first perform exploratory work to experimentally translate instrument settings from legacy to new model, and then we can add replicate testing to build confidence in the new method before it becomes routinely used. The scope of work is customizable to fit the client’s requirements.

PTL typically offers three levels of instrument model related method upgrades to choose from, at three different cost structures:

• A protocol-driven method transfer with repeat testing includes preliminary evaluation of the existing legacy method on the new instrument model, replicate analyses using the new method, statistical evaluation of the results with a comparison to historic method results if available, a copy of the new method, and a protocol and report both formally edited and approved by the client and PTL. The scope of the package is adjustable according to client need.

• A non-protocol-driven method change with repeat testing would include all of the above, but in place of the collaboratively reviewed protocol and report the client receives a PTL-generated standard report of analysis.

• A non-protocol-driven method change would include one analysis using the new instrument method based on PTL SOPs and scientific judgement and a PTL-generated standard report of analysis.

In all cases, the new method aims to maintain the same sample preparation procedures as employed in the legacy method (unless justified and approved by the client), but it adapts instrument settings as appropriate for the new hardware. If the legacy instrument is available at PTL, side-by-side analyses on both instrument models may be performed. Throughout the method change process, PTL standard operating procedures for both instrument operation and method revisions are upheld.

Do keep in mind that if a manufacturer has developed a new instrument model, it will only be a matter of time before the legacy model is removed from their maintenance and support plans. As such, PTL too will have to retire it. As a result, the original method cannot be sustained long-term. We make every effort to contact clients who are affected by these instrument retirements. We want to work with you to make the method change as smooth and scientifically supported as possible.

Contact Particle Technology Labs for more information.

New Advanced Particle Characterization Instrument at Particle Technology Labs

Dynamic Imaging at Particle Technology Labs

Advanced Particle Sizing and Characterization

Particle Technology Labs is pleased to announce the recent installation of our newest dynamic image analyzer; the Malvern (Sysmex) FPIA-3000.
Many times, particle size distribution analysis provides sufficient information about sample material. However, in cases where the shape of raw material particles can affect performance and quality of the end product, more detailed information may be needed. For these applications, automated image analysis provides thorough and accurate particle shape characteristic measurements.

With the ability to analyze tens of thousands of particles per second, this state-of-the-art automated imaging instrument not only measures particle size, but also defines and characterizes particle shape to report detailed variation in particulate.

While instruments such as laser diffractors size particles, it sees them only as spherical. Automated imaging instrumentation has the ability to not only size particles, but also detect and enumerate agglomerates, oversized particles and contaminant particles. It can measure the size of non-spherical particles such as needle-shaped crystals, providing length and width measurements, and can detect physical properties such as transparency. It can also differentiate between individual components within a mixture.

Automated imaging works by using a high-resolution digital camera to capture images of dispersed sample particulate. Using digital thresholding techniques, images of particles are automatically and objectively measured, analyzed and classified for inclusion/exclusion. In reporting, images are displayed together with particle size and shape data, providing a very effective visual verification of results.

Our newest system, the Malvern (Sysmex) FPIA-3000 provides a robust statistical measurement of particles in a sample as a whole. Compared to manual microscopy, automated imaging analyzes a larger amount of sample in a shorter amount of time, reducing operator subjectivity. This leads to more reliable and accurate results.

This new instrument joins PTL's advanced particle characterization automated imaging instrument, the Malvern Morphologi G3 system. Visit our Image Analysis page on our website for more information.

PTL Receives ACIL Customer Quality Service Award for its Fifth Consecutive Year

PTL is proud to receive the ACIL Customer Quality Service Award for the fifth consecutive year.

This program provides users with a mechanism for evaluating testing laboratories.  Participants are committed to ensuring the integrity of data, meeting customer’s quality needs and setting the standards of performance for the testing laboratory industry.
 
Any testing laboratory who wants to be recognized as a participating laboratory must maintain proof of an annual ethics training and an early detection system for questionable analytical practices, submit a signed code of ethics and distribute satisfaction surveys to their customers.
 
The participants have committed to a uniform code of ethics and Customer Survey data for comparison to other participants.  The Customer Quality Service Award participants demonstrate that they are proud of the quality they achieve and always operate with customer service as a top priority.
 
We are pleased to once again qualify into this program. Thank you to all our customers who provided honest feedback regarding our particle characterization services.

Q & A with Shane Hill of PTL’s Method Services Department

The method services business has grown significantly in recent years. PTL is pleased to provide these services to form stronger relationships with our pharmaceutical clients and help them achieve their goals.

At the helm of PTL’s validation department is Shane Hill, Methods Compliance Assistant Manager. Shane took time from his schedule to answer a few questions about the method services available at PTL.

1. What are method developments, method validations, and method transfers, and what does each entail?

A method development is a process whereby an analytical procedure is created for a specified sample type. Clients will either submit a sample with no established test document or they will provide a nominal procedure that covers a given characterization technique (particle sizesurface area, etc.), and PTL will tailor the method through detailed evaluations. A design of experiments (DOE) is then undertaken, during which several method parameters are investigated for their significance in affecting the results. The DOE data are processed via statistical software; the method is updated to incorporate the optimized settings and a proof of concept is executed to demonstrate precision of the new method.

A method validation is a process which is ideally initiated following varying degrees of method development. Validations are intended to demonstrate that an analytical procedure is suitable for a given sample type. For physical analyses, the testing typically consists of accuracy, precision, and robustness. Accuracy serves to illustrate the trueness of the data within the specified range of interest. Precision demonstrates repeatability of generated data; often validation studies at PTL examine precision across multiple days, chemists, and instruments for a comprehensive comparison. Robustness evaluates the impact of small method variations on the final results.  Data are compared against USP acceptance criteria and/or client-provided specifications, as well as processed via statistical software which reports means, equivalencies, and comparative variability.

A method transfer acts as a precision study between instruments, such as when an older generation instrument is retired and a test method requires transferring to a newer generation instrument, or between laboratories. PTL has extensive experience with both scenarios.  Typically, testing is conducted concurrently across instruments/laboratories, and the data are compared against acceptance criteria. Accuracy is often included as a measure of system suitability.

Across all our method services, PTL follows industry and regulatory guidances in the development and execution of the testing.

2.  How long, on average, does each service take to complete?

Method developments take about 3-4 weeks to complete, from initial evaluation to reporting. Method validations take about 4-6 weeks (depending on the inclusion of robustness and sample difficulty). Method transfers take about 3-4 weeks to complete, from protocol creation to reporting.

3. How does each service benefit the client?

Foremost, PTL’s method services help our clients comply with the FDA’s cGMP regulations.  A robust method development ensures that the analytical procedure provides optimized, linear data for the sample material. Method validations benefit our clients by allowing a test procedure to undergo several levels of precision testing to ensure correlation across several variables, such as days, chemists, and instruments. If robustness is evaluated, then there is the added benefit of demonstration of an optimized method. Method transfers allow a test method to seamlessly be updated to a newer, more efficient particle characterization instrument or to PTL if the transfer is from an outside laboratory.

4. Are there any related services that we offer?

In addition to developments, validations, and transfers, PTL also offers method verifications. Often clients will require a test procedure to be verified against a USP Chapter or Monograph; PTL will design a protocol that includes references to the USP guidelines and will perform the verification testing accordingly. Most often this testing includes a repeatability evaluation, but can include more elements depending on the USP Chapter or Monograph involved.

To read more about how PTL’s method services can benefit you, click here.

“We have been working with PTL’s Methods Service Department for many years and the client service has always been great in terms of technical knowledge, answering e-mails promptly, and quick turnaround of quotations and method transfer reports.”  – Rajat Gandhi of CPL, Ltd."

PTL at the US Power Plant Water Treatment Conference

Water is just one of many industries that turn to PTL for expert particle size and characterization testing. Water particulate is tested for many reasons including determining the characteristics for health and environmental purposes. Particle Technology Labs will be attending the US Power Plant Water Treatment conference in Chicago on September 12th and 13th. The conference brings together industry figures within the US power industry to discuss pertinent issues facing water management. For more information about the conference, visit https://www.lmnpower.com/