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 size, surface 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."